药物合成翻译习题答案.docx

In a 3L round-bottomed flask fitted with a reflux condenser are placed 625 mL of 95 percent alcohol, 500 mL of water, 500 g of pure benzaldehyde, and 50 g of sodium cyanide. The mixture is then heated and kept boiling for one-half hour. In the course of about twenty minutes, crystals begin to separate from the hot solution. At the end of the thirty minutes, the solution is cooled, filtered with suction, and washed with a little water. The yield of dry crude benzoin, which is white or light yellow, is 450460 g. In order to obtain it completely pure, the crude substance is recrystallized from 95 percent alcohol, 90 g of crude material being dissolved in about 700 mL of boiling alcohol; upon cooling, a yield of 83 g of white, pure benzoin which melts at 129 C is obtained.(benzoin：安息香胶)在3L圆底烧瓶装上回流冷凝器置于625毫升百分之95酒精，500毫升水，500克和50克的纯甲醛、氰化钠。然后将混合物加热并保持沸腾一个半小时。在大约二十分钟的过程中，晶体开始从热溶液中分离。在三十分钟结束时，该溶液被冷却，用抽吸过滤，用少量的水冲洗。干粗安息香的产量，这是白色或淡黄色，450460 G.为了获得完全纯净，粗品重结晶百分之95酒精、90克粗品溶于约700毫升煮沸酒精；冷却后，产率83克白，得到纯安息香，融化在129C。A dry, 1L, three-necked flask fitted with a sealed mechanical stirrer, a thermometer, and a drying tube, is charged with 500 mL of anhydrous pyridine, which is stirred and cooled to approximately 15 with an ice bath. The drying tube is periodically removed and 68g (0.68 mole) of anhydrous chromium(VI) oxide is added in portions through the neck of the flask over a 30 minute period. As the chromium trioxide is added, an intensely yellow, flocculent precipitate separates from the pyridine and the viscosity of the mixture increases. When the addition is complete, the mixture is allowed to warm slowly to room temperature with stirring. Within one hour the viscosity of the mixture decreases and the initially yellow product changes to a deep red, macrocrystalline form that settles to the bottom of the flask when stirring is discontinued. The supernatant pyridine is decanted and the crystals are washed several times by with 250mL portions of anhydrous petroleum ether. The complex is dried at 10mm until it is free-flowing, leaving 150160g of dipyridine chromium(VI) oxide as red crystals. The product is extremely hygroscopic; contact with moisture converts it rapidly to the yellow dipyridinium dichromate. It is stored at 0 in a brown bottle.干燥，1L，三颈烧瓶中装有一个密封的机械搅拌器，温度计，和干燥管，被指控500毫升无水吡啶，其中搅拌冷却至约15用冰浴。干燥管定期清除和68g（0.68摩尔）无水铬（VI）的氧化物中添加了部分通过瓶颈在30分钟的时间。由于加入了氧化铬，一种强烈的黄色絮状沉淀分离吡啶和混合物的粘度增加。当添加完成后，该混合物可以慢慢地加热到室温，搅拌。一个小时内的混合物的粘度降低，最初黄产品变为深红色，粗晶的形成，沉淀到瓶底时，停止搅拌。上清吡啶倾和晶体是洗几次用无水石油醚部分250ml。复杂的是干在10mm直到它是自由流动的，剩下的150160G的联吡啶铬（VI）氧化为红色晶体。产品极易吸湿；接触水份将迅速向黄双吡啶重铬酸。它储存在一个棕色瓶子里的0个A dry, 1L, three-necked round-bottomed flask is equipped with a mechanical stirrer, and 650 mL of anhydrous dichloromethane is added. Stirring is begun and 0.300 mole of dipyridine chromium(VI) oxide is added at room temperature, followed by 0.050 mole of 1-heptanol in one portion. After stirring for 20 minutes, the supernatant solution is decanted from the insoluble brown gum, which is washed with three 100mL portions of ether. The ether and dichloromethane solutions are combined and washed successively with 300 mL of aqueous 5% sodium hydroxide, 100 mL of 5% hydrochloric acid, two 100 mL portions of saturated aqueous sodium hydrogen carbonate, and, finally, with 100 mL of saturated aqueous sodium chloride. The organic layer is dried over anhydrous magnesium sulfate, and the solvent is removed by distillation. Distillation of the residual oil at reduced pressure separates 4.04.8 g. (7084%) of heptanal.干燥，1L，三颈圆底烧瓶装有机械搅拌器，和650毫升无水二氯甲烷加入。搅拌开始和0.300摩尔的联吡啶铬（VI）的氧化物在室温下加入，其次是0.050摩尔的庚醇中的一部。搅拌20分钟后，倾去上清液与不溶性褐色胶，这与三毫升乙醚部分洗。对乙醚、二氯甲烷溶液结合300毫升5%的氢氧化钠水溶液中依次洗涤，100毫升5%盐酸100 mL，两部分氢气饱和碳酸钠溶液，和，最后，用100毫升的饱和氯化钠水溶液。在无水硫酸镁上干燥有机层，并通过蒸馏除去溶剂。在减压分离44.8克的残余油蒸馏（7084%）对庚醛。A dry, 1L, three-necked flask fitted with a sealed mechanical stirrer, a thermometer, and a drying tube, is charged with 500 mL of anhydrous pyridine, which is stirred and cooled to approximately 15 with an ice bath. The drying tube is periodically removed and 68g (0.68 mole) of anhydrous chromium(VI) oxide is added in portions through the neck of the flask over a 30 minute period. As the chromium trioxide is added, an intensely yellow, flocculent precipitate separates from the pyridine and the viscosity of the mixture increases. When the addition is complete, the mixture is allowed to warm slowly to room temperature with stirring. Within one hour the viscosity of the mixture decreases and the initially yellow product changes to a deep red, macrocrystalline form that settles to the bottom of the flask when stirring is discontinued. The supernatant pyridine is decanted and the crystals are washed several times by with 250mL portions of anhydrous petroleum ether. The complex is dried at 10mm until it is free-flowing, leaving 150160g of dipyridine chromium(VI) oxide as red crystals. The product is extremely hygroscopic; contact with moisture converts it rapidly to the yellow dipyridinium dichromate. It is stored at 0 in a brown bottle.干燥，1L，三颈烧瓶中装有一个密封的机械搅拌器，温度计，和干燥管，被指控500毫升无水吡啶，其中搅拌冷却至约15用冰浴。干燥管定期清除和68g（0.68摩尔）无水铬（VI）的氧化物中添加了部分通过瓶颈在30分钟的时间。由于加入了氧化铬，一种强烈的黄色絮状沉淀分离吡啶和混合物的粘度增加。当添加完成后，该混合物可以慢慢地加热到室温，搅拌。一个小时内的混合物的粘度降低，最初黄产品变为深红色，粗晶的形成，沉淀到瓶底时，停止搅拌。上清吡啶倾和晶体是洗几次用无水石油醚部分250ml。复杂的是干在10mm直到它是自由流动的，剩下的150160G的联吡啶铬（VI）氧化为红色晶体。产品极易吸湿；接触水份将迅速向黄双吡啶重铬酸。它储存在一个棕色瓶子里的0个。A solution of sodium ethoxide (prepared by the addition of 69g sodium to 950 mL of absolute ethanol) is cooled to 0- 5oC in an ice bath and stirred. The stopper is replaced by a dropping funnel, and a cold mixture (5- 15 oC) of 108g of freshly distilled 2-butanone and 482g of diethyl oxalate is added gradually over a period of 30 minutes. After the addition is complete, the thick, orange red mixture is allowed to warm with continued stirring to room temperature, heated under reflux for 30 minutes, and cooled again to 0oC in an ice bath. The mixture is decomposed by stirring with 165 mL of sulfuric acid(1:1 by volume) added in portions. The sodium sulfate formed is filtered by suction and washed with ethanol (150