藥物合成反應(yīng)課后翻譯doc(編輯修改稿)
2025-08-11 06:11 本頁(yè)面
【文章內(nèi)容簡(jiǎn)介】 action mixture is again refluxed for 15 minutes, vigorous stirring being maintained all the while (Note 4). 反應(yīng)物在充分?jǐn)嚢柘轮匦禄亓?5分鐘。The cooled mixture is transferred to a 3l. separatory funnel, and the ethylene dichloride layer is removed. 冷卻的混合物轉(zhuǎn)移到分液漏斗中，出去二氯乙烯層。The aqueous phase is extracted three times with a total of about 500 ml. of ether. 水相用500ml乙醚分三次萃取。The ether and ethylene chloride solutions are bined and washed with three 100ml. portions of saturated aqueous sodium carbonate solution, which is added cautiously at first to avoid too rapid evolution of carbon ，用100ml飽和碳酸鈉溶液分三次洗滌，然后通入二氧化碳，通入時(shí)要小心不要太快。 The non aqueous solution is then dried over anhydrous sodium carbonate, the solvents are distilled, and the remaining liquid is transferred to a Claisen flask and distilled from an oil bath under reduced pressure (Note 5). 非水溶液用無(wú)水碳酸鈉干燥，蒸餾溶劑，余下的溶液移入克氏燒瓶在油浴中減壓蒸餾。The aldehyde boils at 78176。 at 2 mm.。 there is very little forerun and very little residue. 醛沸點(diǎn)78度在2mm；很少有預(yù)留無(wú)和殘?jiān)he yield of crude 2pyrrolealdehyde is 85–90 g. (89–95%), as an almost waterwhite liquid which soon crystallizes. 當(dāng)幾乎透明的液體會(huì)馬上結(jié)晶，粗品產(chǎn)量8590g（8995%）。A sample dried on a clay plate melts at 35–40176。. 樣品在素?zé)砂迳细稍?，熔點(diǎn)3540度。The crude product is purified by dissolving in boiling petroleum ether (. 40–60176。), in the ratio of 1 g. of crude 2pyrrolealdehyde to 25 ml. of solvent, and cooling the solution slowly to room temperature, followed by refrigeration for a few （沸點(diǎn)4060度），一克粗品2甲基吡啶加入25ml溶劑，在室溫下冷卻，這后再冷凍數(shù)小時(shí)。 The pure aldehyde is obtained from the crude in approximately 85% ，收率85%。 The overall yield from pyrrole is 78–79% of pure 2pyrrolealdehyde, . 44–45176。. 總得率為7879%熔點(diǎn)4445度。（1）反應(yīng)式(1)In a 3L. roundbottomed flask (Note 1) fitted with a reflux condenser are placed 625 cc. of 95 per cent alcohol (Note 2), 500 cc. of water, 500 g. (476 cc., moles) of pure benzaldehyde (Note 3), and 50 g. of sodium cyanide (96–98 per cent). 在配有回流冷凝器的3L圓底燒瓶中加入625ml的95%酒精、500ml水、500g（476ml，4,7mol）的苯甲醛和50g 9698%的氰化鈉。The mixture is then heated and kept boiling for onehalf hour (Note 4). 。In the course of about twenty minutes, crystals begin to separate from the hot solution. 在20分鐘后晶體開(kāi)始從熱溶液中析出。At the end of the thirty minutes, the solution is cooled, filtered with suction, and washed with a little water. 在最后的30分鐘，冷卻溶液，抽濾并用少量水洗滌The yield of dry crude benzoin, which is white or light yellow, is 450–460 。 (90–92 per cent of the theoretical amount). 理論產(chǎn)率9092%。In order to obtain it pletely pure, the crude substance is recrystallized from 95 per cent alcohol, 90 g. of crude material being dissolved in about 700 cc. of boiling alcohol。 upon cooling, a yield of 83 g. of white, pure benzoin which melts at 129176。 is ，粗產(chǎn)品要在酒精中重結(jié)晶，90g粗品溶解在700ml沸騰的酒精中，冷卻， 得到83g熔點(diǎn)為129攝氏度的白色安息香純品。(2)In a 1L. threenecked roundbottomed flask equipped with a mechanical stirrer, short reflux condenser, and bent glass tube reaching below the surface of the liquid for the introduction of hydrogen chloride, are placed 50 g. ( mole) of pnitrophe
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