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 aqueou s 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。 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%)白晶体熔点137–140°C Preparation of mesitaldehyde (2,4,6- trimethyl benzaldehyde) 2,4,6-拉挤模具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地震云与地震预测
5分钟，移开冰浴反应30永磁接触器分钟，再在35℃下反应15分钟。 The 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 数字迎新系统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）。
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 a mercury-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。The solution is cooled to 0–5° in an ice bath and stirred.溶液在0-5℃下冰浴搅拌。 The stopper is replaced by a dropping funnel, and a cold mixture (5–15°) of 108 g. (1.50 moles) of freshly distilled 2-butanone a
nd 482 g. (3.30 moles) of diethyl oxalate (Note 1) is added gradually over a period of 30 minutes.瓶塞用分液漏斗取代，108g（1.5mol）的丁二酮和482g（3.3mol）的乙二酸二乙酯在5-15℃下低温混合，在30分钟内逐步滴加到溶液中。 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 0° in an ice bath. 完全加入后，橘红的粘稠物继续搅拌至室温，加热回流30分钟后在冰浴中冷却至0℃。The mixture is decomposed by stirring with 165 ml. of sulfuric acid (1:1 by volume) added in portions.将165ml浓硫酸（体积比1:1）在搅拌加入，分解混合物。 The sodium sulfate formed is filtered by suction and washed with ethanol (150–200 ml.) (Note 2). 硫酸钠抽滤后用乙醇（150–200 ml）洗涤。The washings and filtrate are combined and concentrated by evaporation .合并滤液和洗涤液后蒸发浓缩。耐高温防爆玻璃The yellowish brown product which accumulates by slow crystallization is collected by filtration, washed with small quantities of ice-cold water, and dried in air. 过滤缓慢析出的棕黄产品用小剂量的冰水洗涤后在空气中干燥。空间种植塔 The crude product weighs 140–150 g.粗产品140-150g。 Further evaporative concentration of the mother liquor followed by cooling furnishes an a
dditional 40–50 g. of the keto ester, 此外将母液用冷冻蒸发浓缩后又得到40-50g的酮酯。bringing the total yield to 180–200 g. (53–59%)产品总共180-200g（产率53-59%） (Note 2). This crude material (m.p. 120–130°) is used in the next step.粗品（熔点120–130℃）用于下一步中 A pure sample can be obtained by crystallization from ethyl acetate after treatment with Norit activated carbon, m.p. 160–162°.纯品是经过活性炭处理后在乙酸乙酯中结晶得到，熔点160–162℃。
The procedure for 2- pyrrolealdehyde 2-吡咯甲醛
In a 3-l. three-necked round-bottomed flask, fitted with a sealed stirrer, a dropping funnel, and a reflux condenser, is placed 80 g. (1.1 moles) of dimethylformamide (Note 1).在配有封闭搅拌器、滴液漏斗和冷凝回流装置的三口圆底烧瓶中放入80g（1.1mol）的二甲基甲酰胺。 The flask is immersed in an ice bath, and the internal temperature is maintained at 10–20°, while 169 g. (1.1 moles) of phosphorus oxychloride is added through the dropping funnel over a period of 15 minutes. 烧瓶浸入冰浴中，内部温度保持在10-20℃，169g（1.1mol）的磷酰氯通过滴液漏斗在15分钟内滴加。An exothermic reaction occurs
with the formation of the phosphorus oxychloride - dimethylformamide complex. 放热反应生成磷酰氯二甲基甲酰胺化合物。The ice bath is removed, and the mixture is stirred for 15 minutes (Note 2). 移去冰浴，在搅拌15分钟。
The ice bath is replaced, and 250 ml. of ethylene dichloride is added to the mixture. 重新再冰浴下加入250ml的二氯乙烯。When the internal temperature has been lowered to 5°, a solution of 67 g. (1.0 mole) of freshly distilled pyrrole in 250 ml. of ethylene dichloride is added through a clean dropping funnel to the stirred, cooled mixture over a period of 1 hour. 当内部温度降到5度时，把67g（1.0mol）新蒸馏的吡咯加入到250二氯乙烯中，通过滴液漏斗在1小时内低温下边搅拌边滴加。After the addition is complete, the ice bath is replaced with a heating mantle, and the mixture is stirred at the reflux temperature for 15 minutes, during which time there is copious evolution of hydrogen chloride.滴加完后，用加热装置取代冰浴，搅拌回流15分钟， 直到有大量氯化氢产生。
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