药物合成反应(第三版)第二章课后翻译
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1、216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
Near the end of the addition, the mass becomes molten and can be stirred easilygrams of heavy dark residue by distillation at reduced pressure. 乙醚在常压下蒸馏,微量的溴苯乙酮通过减压蒸馏的方法从大量深色残渣中被分离出来。
The colorless distillate is carefully fractionated to obtain 94–100 g.通过分馏,得到无色的流出液94-100g2、反应式:3、2-Methyl-4-ethoxalylcyclopentane-1,3,5-trione. A solution of sodium ethoxide is prepared in a 2-l. three-necked, round-bottomed flask fitted with amercury-sealed stirrer, a reflux condenser carrying a drying tube, and a stopper by the addition of 69.0 g. (3 moles) of sodium to 950 ml. of absolute ethanol. 69.0g (3mol)钠和950ml无水乙醇在配有干燥回流冷凝管和汞封搅拌器的2L三口圆底烧瓶中制备乙醇钠。
1、About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1、About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g–moles)的无水三氯化铝。
Whilefrom the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
Near the end of the addition, the mass becomes molten and can be stirred easily without being明苯乙酰已经和三氯化铝混合完全,颜色也逐渐从黄褐色变为棕色。
Bromine (128 g., mole) is added dropwise to the well-stirred mixture over a period of 40 minutes (Note 4). 在40分钟内在搅拌下把溴缓慢滴加到混合物中。
1、About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1、About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1、216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
Near the end of the addition, the mass becomes molten and can be stirred easilygrams of heavy dark residue by distillation at reduced pressure. 乙醚在常压下蒸馏,微量的溴苯乙酮通过减压蒸馏的方法从大量深色残渣中被分离出来。
The colorless distillate is carefully fractionated to obtain 94–100 g.通过分馏,得到无色的流出液94-100g2、反应式:3、2-Methyl-4-ethoxalylcyclopentane-1,3,5-trione. A solution of sodium ethoxide is prepared in a 2-l. three-necked, round-bottomed flask fitted with amercury-sealed stirrer, a reflux condenser carrying a drying tube, and a stopper by the addition of 69.0 g. (3 moles) of sodium to 950 ml. of absolute ethanol. 69.0g (3mol)钠和950ml无水乙醇在配有干燥回流冷凝管和汞封搅拌器的2L三口圆底烧瓶中制备乙醇钠。
四次把深色的油从混合物中用 150ml 萃取岀来。
The extracts are combined, washedto produce a temperature above 180° .然而,速度不能太快,当反应温度超过either heated or cooled. The molte n mass, in which the acet ophenon e is complexed with aluminum chloride, ranges in color from tan to brown.明苯乙酰已经和三氯化铝混合完全,颜色也逐渐从黄褐色变为棕色。
混合均匀。
Part of the cold aqueous layer is added to the reacti on flask to deco mposewhatever part of the reactionmixture remains there, and the resultingmixture is addedto the beaker.把部分的冰水层加入到烧瓶中洗涤残留物,然后合并到烧杯中。
that settles out is extracted from the mixture with four 150-ml. p orti ons of etherAbout 216 — 224 g. — moles) of po wdered an hydrous aluminum chloride is added to a1Lthree-necked flask.在1L 的三口烧瓶中加入大约 216-224g - moles)的无水三氯化铝。
While the freeflow ing catalyst is stirred (Note 3), 81 g. mole) of acet ophenone is added from the dropping funnel in a slow stream over a p eriod of 20 -30 minutes. 自由流动 的催化剂边搅拌边用滴液漏斗缓慢滴加 81g 苯乙酰。
1、216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
Near the end of the addition, the mass becomes molten and can be stirred easilygrams of heavy dark residue by distillation at reduced pressure. 乙醚在常压下蒸馏,微量的溴苯乙酮通过减压蒸馏的方法从大量深色残渣中被分离出来。
The colorless distillate is carefully fractionated to obtain 94–100 g.通过分馏,得到无色的流出液94-100g2、反应式:3、2-Methyl-4-ethoxalylcyclopentane-1,3,5-trione. A solution of sodium ethoxide is prepared in a 2-l. three-necked, round-bottomed flask fitted with amercury-sealed stirrer, a reflux condenser carrying a drying tube, and a stopper by the addition of 69.0 g. (3 moles) of sodium to 950 ml. of absolute ethanol. 69.0g (3mol)钠和950ml无水乙醇在配有干燥回流冷凝管和汞封搅拌器的2L三口圆底烧瓶中制备乙醇钠。
药物合成反应方程式第一章:卤代反应1.2.3.4.5.6.第二章:烃化反应1.盐酸普萘洛尔的合成:2.盐酸氯丙嗪的合成:构型保持构型反转4.第三章:酰化反应 1. 2. 3. 4第四章:缩合反应 1. 2. 3 4.6.7.8.9.10.11. 13.第五章:重排反应1.2.3.4.5.7.8.9. 11.12.13.14.15.17.第六章:氧化反应 一、完成下列反应: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.℃℃11.12.13.14.二、写出下列反应的主要试剂和反应条件:1.2. 3.4.5.6.7.8.9.第七章:还原反应 一、完成下列反应: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.二、写出下列反应的化学试剂和反应条件: 1.2.3.4.5. 其他:1.在利尿药氯噻酮的中间体对氯苯甲酸的制备中,为什么1mol的邻苯二甲酸酐要用2.4mol的AlCl3为催化剂?若傅克酰化反应中用酰氯为酰化剂,催化剂AlCl3的用量如何?反应结束后,产物如何从反应中分离?2.下列两种甾醇以鉻酸氧化时,哪一种速度快,为什么?药物合成名词解释1.Adams’ catalyst (Adams催化剂):将氯铂酸铵与硝酸钠混合均匀后灼热熔融,氧化过程中有大量二氧化氮放出,经洗涤等处理后即得二氧化铂催化剂。
2.Arndt-E istert reaction (Arndt-E istert重排):Arndt-Eistert等用酰氯与重氮甲烷反应得α-重氮酮,再经Wollf重排,生成比原酰氯多一个碳的羧酸,该反应环称Arndt-Eistert反应。
3.Baeyer-Villiger oxidation (Baeyer-Villiger氧化反应):在酸催化下,醛或酮与过氧酸作用,在烃基与羰基之间插入氧生成酯的反应称为Baeyer-V illiger氧化重排。
4.Beckmann rearrangement (Beckmann重排):醛肟或酮肟在酸性催化剂作用下重排成取代酰胺的反应称Beckmann重排。
药物合成反应与设计翻译部分(第三版闻韧主编)第一章翻译:About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1、About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1、About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1、216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst isfunnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
Near the end of the addition, the mass becomes molten and can be stirred easily without being either heated or cooled. The molten mass, in which thebrown.当快滴加完时,团块开始融化,表明苯乙酰已经和三氯化铝混合完全,颜色也逐渐从黄褐色变为棕色。
1、About 216–224 g. (1.62–1.68 moles) of powdered anhydrous aluminum chloride is added to a 1Lthree-necked flask.在1L的三口烧瓶中加入大约216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst is stirred (Note 3), 81 g. (0.67 mole) of acetophenone is added from the dropping funnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能被分散,就会变黑或是碳化。
When about one-third of the acetophenone has been added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
1、216-224g(1.62–1.68 moles)的无水三氯化铝。
While the free-flowing catalyst isfunnel in a slow stream over a period of 20–30 minutes. 自由流动的催化剂边搅拌边用滴液漏斗缓慢滴加81g苯乙酰。
Considerable heat is evolved, and, if the drops of ketone are not dispersed, darkening or charring occurs. 放热反应,假如滴加的酮不能added, the mixture becomes a viscous ball-like mass that is difficult to stir.当三分之一的乙酰苯被滴加,反应混合物变成一个很难搅拌的粘性的球状团块。
Turning of the stirrer by hand or more rapid addition of ketone is necessary at this point. 在这时,改用手动搅拌或快速滴加酮是非常必要的。
The addition of ketone, however, should not be so rapid as to produce a temperature above 180°. 然而,速度不能太快,当反应温度超过180℃时。
Near the end of the addition, the mass becomes molten and can be stirred easily without being either heated or cooled. The molten mass, in which thebrown.当快滴加完时,团块开始融化,表明苯乙酰已经和三氯化铝混合完全,颜色也逐渐从黄褐色变为棕色。
第二章课后翻译
Preparation of cyclopropane 1,1- dicarboxylic acid环丙烷1,1-二甲酸的制备(1). To a 1-L solution of aqueous 50% sodium hydroxide(Note 1), mechanically stirred in a 2-L, three-necked flask, was added, at 25°C, 114.0 g (0.5 mol) of triethylbenzylammonium chloride(TEBA三乙基苄基氯化铵)(Note 2).1L的50%氢氧化钠加入到2L的三口烧瓶中,加入TEBA三乙基苄基氯化铵114.0g(0.5mol)在25℃机械搅拌。
To this vigorously stirred suspension was added a mixture of 80.0 g (0.5 mol) of diethyl malonate and 141.0 g (0.75 mol) of 1,2-dibromoethane all at once.充分搅拌至混悬状,一次性加入丙二酸二乙酯80.0g(0.5mol)和1,2-二溴乙烷141.0个(0.75mol)的混合物。
The reaction mixture was vigorously stirred for 2 hr (Note 3).反应混合物强烈搅拌2小时。
The contents of the flask were transferred to a 4-L Erlenmeyer flask by rinsing the flask with three 75-mL portions of water.把烧瓶中的物质转移到4L的锥形瓶中,并用75ml清水洗涤烧瓶三次。
The mixture was magnetically stirred by dropwise addition of 1 L of concentrated hydrochloric acid.混合物在磁力搅拌下缓慢滴加浓盐酸。
The temperature of the flask was maintained between 15 and 25°C during acidification. 在酸化过程中烧瓶内的温度保持在15-25℃之间。
The aqueous layer was poured into a 4-L separatory funnel and extracted three times with 900 mL of ether.反应物的水层在4L的分液漏斗中用900ml乙醚分三次萃取。
The aqueous layer was saturated with sodium chloride and extracted three times with 500 mL of ether.水层用氯化钠饱和,并且用500ml乙醚分三次萃取。
The ether layers were combined, washed with 1 L of brine, dried (MgSO4), and decolorized with activated carbon.合并乙醚液,用浓盐水洗涤,干燥,用活性炭脱色。
Removal of the solvent by rotary evaporation gave 55.2 g of a semisolid residue.用旋转蒸发器出去溶剂得55.2g的半固体。
The residue was triturateed with 100 mL of benzene.残渣用100ml苯磨碎。
Filtration of this mixture gave 43.1–47.9 g (66–73%) of 1 as white crystals, mp 137–140°C.过滤的混合物为43.1-47.9g(66–73%)白色晶体熔点137–140°C
Preparation of mesitaldehyde (2,4,6- trimethyl benzaldehyde) 2,4,6-三甲基苯甲醛的制备
A solution of 72 g. (0.60 mole) of mesitylene in 375 ml. of dry methylene chloride is placed in a 1-l. three-necked flask equipped with a reflux condenser, a stirrer, and a dropping funnel. 72g (0.60mol)的1,3,5-三甲基苯和无水的二氯甲烷放入配有冷凝回流、搅拌和滴液漏斗装置的三口烧瓶中。
The solution is cooled in an ice bath, and 190 g. (110 ml., 1.0 mole) of titanium tetrachloride is added over a period of 3 minutes. 在冰浴的条件下,在三分钟内滴加190g (110ml,1.0mol)的四氯化钛。
While the solution is stirred and cooled, 57.5 g. (0.5 mole) of dichloromethyl methyl ether 2 is added dropwise over a 25-minute period.之后再冰浴和搅拌下,在25分钟内滴加57.5g(0.5mol)滴加二氯甲基甲醚。
The reaction begins (as indicated by evolution of hydrogen chloride) when the first drop of chloro ether is added. 当开始滴加氯代醚,则反应开始(有氯化氢放出)After the addition is complete, the mixture is stirred for 5 minutes in the ice bath, for 30 minutes without cooling, and for 15 minutes at 35°.在滴加完成后,混合物在冰浴下搅拌5分钟,移开冰浴反应30分钟,再在35℃下反应15分钟。
Th e reaction mixture is poured into a separatory funnel containing about 0.5 kg. of crushed ice and is shaken thoroughly.反应混合物移入分液漏斗,并加0.5kg的碎冰,充分振摇。
The organic layer is separated, and the aqueous solution is extracted with two 50- ml. portions of
methylene chloride.弃去有机层,水层再用50ml的二氯甲烷分两次萃取。
The combined organic solution is washed three times with 75-ml. portions of water.合并萃取液,用75ml水分三次洗涤。
A crystal of hydroquinone is added to the methylene chloride solution (Note 1) which is then dried over anhydrous sodium sulfate. 对二苯酚晶体加入到二氯甲烷溶液中,在加入无水硫酸钠干燥。
After evaporation of the solvent, the residue is distilled to give the crude product, b.p. 68–74° (0.9 mm.).蒸去溶剂便得到粗品沸点68-74℃(0.9mm)After redistillation there is obtained 60–66 g. (81–89%) of mesitaldehyde; b.p. 113–115° (11 mm.), n20D 1.5538.重蒸馏得到60-66g(81-89%)的2,4,6-三甲基苯甲醛沸点113-115℃(11mm)。