药物合成反应(第三版)第一,二 三章课后翻译

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药物合成之缩合反应翻译

药物合成之缩合反应翻译

药物合成反应——缩合反应翻译一、In a 3L round-bottomed flask with a reflux condenser are placed 625mL of 95 percent alcohol, 500mL of water, 500g (476ml, 4.7mol) of pure benzaldehyde, and 50g of sodium cyanide (96-98 percent). 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 thirty minutes, the solution is cooled, filtered with suction, and washed with a little water. The yield of the dry crude benzoin, which is white or light yellow, is 450-460g (90-92 percent of the theoretical amount). In order to obtain it completely pure, the crude substance is recrystallized from 95 percent alcohol. 90g of crude material being dissolved in about 700ml of boiling alcohol; upon cooling, a yield of 83g of white, pure benzoin which melts at 129℃is obtained.二、In a 1L three-necked round-bottomed flask equipped with mechanical stirrer, short reflux condenser, and bent glass tube reaching below the surface of the liquid for the introduction of hydrogen chloride, are placed 50g(0.36mol) of p-nitrophenol, 650ml of concentrated hydrochloric acid, 5ml concentrated sulfuric acid, and 76g(1mol) of methylal. The mixture is stirred while the temperature is maintained at 70±2℃for 4-5 hours by means of a water bath. During this time hydrogen chloride is bubbled into the reaction mixture through the bent glass tube, and the excess gas is carried away through the refluxcondenser to a hood or gas absorption trap. The 2-hydroxy-5-nitrobenzyl chloride begins to separate as a solid about 1 hour after the beginning of the reaction. At the end of the mixture is cooled in ice for 1 hour whereby more crystals separate, after which the acid liquors are either filtered or decanted from the crystal. The 2-hydroxy-5-nitrobenzyl chloride is purified by recrystallization from 125ml of hot benzene. The yield is 46g (69% based on p-nitrophenol) of a white product melting at 129-130.翻译为:一、在一个3L圆底烧瓶中加入650mL 95%的乙醇,500mL水,476mL苯甲醛,50gNaCN(96-98%)并装上冷凝回流装置.混合物保持沸腾1个半小时,正常情况下大约20分钟有晶体从溶液中析出来。

《药物合成反应》第3章酰化反应

《药物合成反应》第3章酰化反应
回流
CH3
O
C3H7
C CH3
OH +
C C O O
O C O
Et3N TEA
CH3 C C3H7
CH3 C O OH
H3C N CH 3
DMAF:对 二 甲 氨 基 吡 啶
30
混合酸酐的应用 ①羧酸 - 三氟乙酸混合酸酐(适用于立体位阻较大的羧酸的 酯化)
O R C O
H
R
O R C
O
C
O
F3C C O F3C C
HN HN
13
CH3 COOH + H3CO OH
H2C HO CH CH3
CH3
DCC/Et2O R.T.20min
COO CH OH
H2C
CH3
酰化能力弱,因为可形成分子内氢键 CH3 C H3CO OH OH O
H3CO
14
例:
O O
CH2OH
COOH
+
I
DCC/DMAP 25℃
O CH2 O C O O I 96%
(1)增加反应物浓度 (2)不断蒸出反应产物之一 (3)添加脱水剂或分子筛除水。(无水 CuSO4, 无水AI2(SO4)3,(CF3CO)2O,DCC。)
加快反应速率:(1)提高温度 (2)催化剂(降低活化能)
8
醇的结构对酰化反应的影响 立体影响因素:伯醇>仲醇>叔醇
R O
立体效应
R R
C
C
OH
C
R C
28
O N C H
O CH3 + OH C CH3
NH2 H3C C O +
H3C C
O
O

(完整word版)药物合成反应(闻韧_第三版)课后翻译(word文档良心出品)

(完整word版)药物合成反应(闻韧_第三版)课后翻译(word文档良心出品)

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。

闻韧版 药物合成反应 课后翻译

闻韧版 药物合成反应 课后翻译
在反应开始后的一个小时,2-羟基-5-硝基苯氯化物作为固体被分离。最后把混合物在冰中冷却1小时,使更多的晶体析出,之后把酸性液体过滤或倾析得到晶体。2-羟基-5-硝基苯氯化物在热的苯中重结晶纯化。白色产物46g(对硝基苯酚含69%)熔点129-130度
第六章
(1)、二吡啶三氧化铬
在一个干燥的装有密封机械搅拌器,温度计,和干燥管的1L的三颈烧瓶里面装入500毫升无水吡啶,搅拌,用冰浴冷却到大约15°。干燥管是定期拿开,将68克(0.68摩尔)无水三氧化铬在一个30分钟内通过瓶颈分次加入。氧化铬应增加在这样的速度,温度不超过20°,并以这种方式,迅速与吡啶氧化物混合,不粘附瓶内。随着氧化铬的加入,一种深黄色的,絮状沉淀物从吡啶中分离出来,混合物的粘度增加。当添加完后,这混合物
第四章
(1)、 在配有回流冷凝器的3L圆底烧瓶中加入625ml的95%酒精、500ml水、500g(476ml,4,7mol)的苯甲醛和50g 96-98%的氰化钠。混合物加热并保持沸腾1.5小时。在20分钟后晶体开始从热溶液中析出。在最后的30分钟,冷却溶液,抽滤并用少量水洗涤有450-460g白色或亮黄色的干燥的安息香。理论产率90-92%。为了得到纯度高的产品,粗产品要在酒精中重结晶,90g粗品溶解在700ml沸腾的酒精中,冷却, 得到83g熔点为129摄氏度的白色安息香纯品。
合并二氯甲烷溶液_可用稀盐酸,碳酸氢钠溶液和水洗涤,或直接通过助滤剂过滤,或通过色谱柱去除吡啶铬盐_痕迹。去除二氯甲烷获得该产品;少量残余吡啶可通过减少压力下去除。
(3)庚醛
在一个干燥,1L的装有机械搅拌器的三颈烧瓶中加入650ml无水二氯甲烷。开始搅拌,在室温下加入77.5g二吡啶三氧化铬,再一次性加入5.8g 1-庚醇。搅拌20分钟后,倒出上层溶液从这不溶性棕色胶状物中,并用3个100ml乙醚冲洗。乙醚和二氯甲烷的溶液相结合,并先后用300毫升5%氢氧化钠的水,100毫升5%的盐酸(注12),两个100毫升部分饱和碳酸氢钠,并最后用100毫升饱和氯化钠水溶液冲洗。无水硫酸镁干燥有机层,并通过蒸馏去除溶剂。在残余油通过Claisen缩合____减压蒸馏分离4.0-4.8克。 (70-84%)的庚醛,B.P. 80-84°(65毫米),n25D1.4094

《药物合成反应》-闻韧主编第三章酰化反应-知识点总结

《药物合成反应》-闻韧主编第三章酰化反应-知识点总结

#2.11打卡# 完成学习目标第三章酰化反应Acylation Reaction1 定义:有机物分子中O、N、C原子上导入酰基的反应.2 分类:根据接受酰基原子的不同可分为:氧酰化、氮酰化、碳酰化3 用途:药物本身有酰基活性化合物的必要官能团结构修饰和前体药物羟基、胺基等基团的保护。

酰化机理:加成-消除机理加成阶段反应是否易于进行决定于羰基的活性:若L的电子效应是吸电子的,不仅有利于亲核试剂的进攻,而且使中间体稳定;若是给电子的作用相反。

根据上述的反应机理可以看出,作为被酰化物质来讲,无疑其亲核性越强越容易被酰化。

具有不同结构的被酰化物的亲核能力一般规律为;RCH2->R—NH->R—O->R—NH2>R—OH。

在消除阶段反应是否易于进行主要取决于L的离去倾向:L-碱性越强,越不容易离去,Cl- 是很弱的碱,-OCOR的碱性较强些,OH-、OR-是相当强的碱,NH2-是更强的碱。

RCOCl>(RCO)2O>RCOOH 、RCOOR′ >RCONH2>RCONR2′R: R为吸电子基团利于进行反应;R为给电子基团不利于反应R的体积若庞大,则亲核试剂对羰基的进攻有位阻,不利于反应进行酸碱催化碱催化作用是可以使较弱的亲核试剂H-Nu转化成亲核性较强的亲核试剂Nu-,从而加速反应。

酸催化的作用是它可以使羰基质子化,转化成羰基碳上带有更大正电性、更容易受亲核试剂进攻的基团,从而加速反应进行。

氧原子的酰化反应是一类形成羧酸酯的反应,是羧酸和醇的酯化反应,是羧酸衍生物的醇解反应醇的结构对酰化反应的影响伯醇(苄醇、烯丙醇除外)>仲醇>叔醇1) 羧酸为酰化剂:提高收率:(1)增加反应物浓度(2)不断蒸出反应产物之一(3)共沸除水、添加脱水剂或分子筛除水。

(无水CuSO4,无水Al2(SO4)3,(CF3CO)2O,DCC。

)加快反应速率:(1)提高温度(2)催化剂(降低活化能)催化剂(1)质子酸催化法: 无机酸:浓硫酸,氯化氢气体,有机酸:苯磺酸,对甲苯磺酸等。

药物合成反应(第三版)第三章课后翻译

药物合成反应(第三版)第三章课后翻译

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。

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 and 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,橘红色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℃。

药物合成反应(第三版_闻韧)第一章卤化反应

药物合成反应(第三版_闻韧)第一章卤化反应
碳正离子的稳定性:叔>仲>伯 连有烷基、烷氧基、苯基等给电子基团的烯键 碳原子是卤负离子优先进攻的位置。
Organic Reactions for Drug Synthesis
例1.
C6H5 H
CC
H
COOC2H5
Br2 / CCl4
Br
C6H5
C
H C
H Br COOC2H5
C6H5 H CC
H Br COOC2H5
1. 卤素与烯烃的亲电加成反应
(1)反应历程: 第一步:卤正离子向π 键进攻,形成三员环卤正离子 或开放式碳正离子的过渡态。
R1 R3
R2
R4
δ +δ XX
Organic Reactions for Drug Synthesis
R1 R3 CC
R2 X R4
(1)
R1 R3
CC
R2
X R4
(2)
第二步:
反应类型
亲电加成 亲电取代 亲核取代 自由基反应
Organic Reactions for Drug Synthesis
常用的卤化剂 卤素(X2):Cl2、Br2
次卤酸(HOX):HOCl、HOBr
N-卤代酰胺:
如 N-溴(氯)代乙酰胺( NBA,NCA) N-溴(氯)代丁二酰亚胺(NBS,NCS)
Ph H CC
H CH3
NBS / DMSO / H2O
OH
Ph
H
CC
H
Br CH3
NBS / 干燥的DMSO
O H
Ph C C Br CH3
Organic Reactions for Drug Synthesis
五、卤化氢与烯烃的加成

药物合成反应(第三版)第一章课后翻译

药物合成反应(第三版)第一章课后翻译

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。

药物合成反应课后翻译

药物合成反应课后翻译

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。

药物合成反应(第三版_闻韧)第三章 酰化反应

药物合成反应(第三版_闻韧)第三章 酰化反应

Organic Reactions for Drug Synthesis
例:抗胆碱药溴美喷酯(宁胃适)的合成
O C OH
HO CH3CH2ONa N CH3
60-80℃,45min
C-OCH2CH3 +
C OH
O C-O N CH3
O CH3Br C OH C-O N CH3 · Br CH3 (77%)
n-C4H9 CH Zn 175℃
2+
R'OH
O RCOR'
n-C4H9 n-C18H37 C COOH + H3C C
CH2 CH3
n-C18H37 C
COO C
n-C7H15 n C18H37 OH/H △ ,6min
+
n-C7H15 n-C4H9 COO C18H37-n + O H3C C CH3

Organic Reactions for Drug Synthesis
叔醇的酯化:SN1机理。
Organic Reactions for Drug Synthesis
SN1
O ' R-C-L

O R-OH + R'-C
O R'-C + L O 快 R'-C-OR
SN2
O ' R-OH + R-C-L O ' + L R-O--C-R H
n-C18H37 C
n-C7H15
Organic Reactions for Drug Synthesis
3、酸酐为酰化剂
•与酸和酯作酰化剂相比,酸酐的酰化活性较强, 而且酰化反应是不可逆的。 •酰化反应过程可以被酸(硫酸等质子酸以及三氟 化硼等Lewis酸)和碱(主要为醋酸钠以及三乙胺 等有机碱)所催化。 •当酸酐难于制备时,也可采用混酸酐法。常用 的混酸酐有磺酸酐、磷酸酐和碳酸酐。

药物合成反应 第一章 卤化反应

药物合成反应 第一章 卤化反应
(84~85%)
对于环烯、桥卤正离子在位阻小的一面形成:
Me Br
OH H Br
甾体化合物
Me
Br
OH
H Br
84-85%
④有重排产物生成,生成更稳定的C 离子 +
Br2 Ph3CCHCH2 CCl4
Ph3CCH CH2Br+Ph2C C CH2BrBrPh70%23%
δ+ δ δ+ δ Ph3CCH CH2+Br Br
N B S /D M S O
O
r.t
(90%)
O g lu A c 4
OAc Br
O
O
O g lu A c 4
四、卤化氢对不饱和烃的加成反应
• 1. 卤化氢对烯烃的加成 • (1)反应通式
• 通卤化氢气体或其饱和有机溶剂,若困难 ,可加Lewis Acid或密封管加热。
• (2)反应机理 • ①离子对过渡态 • ②三分子协同 • ③自由基加成
• (3)影响因素 • 同离子效应,可减少副反应
• (4)应用特点
• 应用烯烃直接制备二卤代烯,困难。炔烃 的卤加成,方便。
二、不饱和羧酸的卤内酯化反应
• (1)反应通式
(2)反应机理
I2 /K I/N a H C O 3 C H2C O 2H H2O /r.t.4h
O
C
H2C
O
I HH
** O O
目录
第一章 第二章 第三章 第四章 第五章 第六章 第七章
卤化反应 烃化反应 酰化反应 缩合反应 重排反应 氧化反应 还原反应
第一章 卤化反应
有机化合物分子中引入碳—卤键 的反应。包括: 亲电加成、亲电取 代、亲核取代及自由基反应(从 机理上考虑)

药物合成反应(第三版)

药物合成反应(第三版)

Br
Br
Br
Br
(选 择 性 溴 化 试 剂 )
第三节 羰基化合物的卤代反应
一、醛酮α-位氢的卤代反应
选择性溴化剂
O CH3 O Br Br O O Br CH3 CH3 CH3 O CH-Ar Br O CH-Ar
第一节 不饱和烃的卤加成反应
• 加卤素
C C X2 C X C X
概述
X2=Cl2, Br2
• 加卤化氢
C C HX C H C X HX=HCl, HBr, HI
无过氧化物 CH3CH=CH2
CH3CHBrCH3
Markovnikov加 成 反Markovnikov加 成
过氧化物
CH3CH2CH2Br
一、醛酮α-位氢的卤代反应
1,3二羰基化合物
O O H3C C CHCCH3 Cl
O
O
H3C C CH2CCH3
CF3SO2Cl Et3N
第三节 羰基化合物的卤代反应
一、醛酮α-位氢的卤代反应
α-羰基自由基取代
O
游离基反应促进剂 选择性地对烷基取代较多的α -H进行溴代
O Br C R''' R''
E π-络 合 物
X+-X-
H X -H+
σ-络 合 物
CH3 CH3 Cl + CH3 2mol Cl CH3 Br2 /Fe Br + Br CH3 Cl Cl
X
H
CH3
Cl2 /Fe

+
第二节 烃类的卤代反应
二、芳烃卤代反应(亲电取代)
OH H2O 3Br2 OH H2O 2Br2 Br
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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°CPreparation 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 ofmethylene 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)。

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。

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 and 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,橘红色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℃。

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