定制各类格氏试剂

问题:请高手翻译
类型:求助 (悬赏分:3分)
提问:rareearth
等级:
版块:有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
信誉:76%
回复:9
阅读:691
时间:2006-04-15 11:10:26  编辑    加入/取消收藏    订制/取消短消息    举报该贴    

Di-p-tolyl Succinate.-Succinic acid (11 g., 0.09 inole) and
p-cresol (20 g., 0.18 mole) were placed in a 200-ml. roundbottom
flask equipped with a thermometer and a reflux
condenser protected by a drying tube. The flask and contents
were heated to 115-120" by means of an oil-bath.
Phosphorus oxychloride (16 g., 0.1 mole) was added clropwise
to the hot mixture. Toward the end of the addition
the vigorous bubbling due to the evolution of hydrogen
chloride subsided, and on continued heating only a negligible
amount of bubbling was observed. After heating for two
to three hours at 115-120°, the dark reaction mixture was
allowed to cool, whereupon a reddish-brown crystalline
material formed on top of a black viscous material. The
crystalline material was scraped away from the black resin
and mixed with 250 g. of a 1 : 1 mixture of ice and water.
The dark orange crystals were then filtered, dried, and recrystallized
from ethanol to give 17 g. (63.4%) of a light
orange crystalline material, m.p. 114-1 18'. This material
was pure enough to be used in the Fries rearrangement.
Three additional recrystallizations from ethanol afforded a
white crystalline material, m.p. 119-12O0
l-Hydroxy-4-methylanthraquinone.-An attempted rearrangement
of di-p-tolyl phthalate (3.5 g., 0.01 mole) was
carried out as described above for di-p-tolyl succinate, except
that the temperature was held at 100" for 16 hours.
After the chlorobenzene was removed by steam distillation,
a red-brown solid remained in the distillation flask. This
solid was collected and recrystallized from glacial acetic
acid to give I-hydroxy-4-methylanthraquinone as redbrown
needles; yield 0.53 g. (14%), m.p. 171-172'. A
further recrystallization of a sample of this crude product
from ethanol gave bright orange-yellow needles, m.p. 173",
reported** m.p. 175-176'
回复人:tangyyer,★★★★★ (有空来逛逛my blog: http://tangyyer.blog.hexun.com) 时间:2006-04-15 11:57:26   编辑 1楼
整篇都不能翻译吗?还是只是有一点翻译不出来?只需把难点拿出来求助,这样才好得到回复


回复人:readpen, (相信自己 相信明天) 时间:2006-04-15 12:57:19   编辑 2楼
太长了!


回复人:xmn78,▲▲ () 时间:2006-04-15 13:28:05   编辑 3楼
此文献应该很老了.因为把实验操作都说的很详细.其实工艺很简单.一会我给你翻译,那些用多大的反应瓶等简单的操作就忽略了(懒得打字).只要你是做合成的应该一看就懂.

少等,先开会.


回复人:乙酸乙酯,▲▲▲▲ (精细有机中间体) 时间:2006-04-15 15:34:13   编辑 4楼
buneng 不能什么都叫别人干吧??



回复人:xmn78,▲▲ () 时间:2006-04-15 15:55:11   编辑 5楼
1.琥珀酸二对甲苯酯
琥珀酸(11 g., 0.09 inole),对甲苯酚(20 g., 0.18 mole)加入200ml反应平中,装回流管,升至115-120度,滴加三氯氧磷(16 g., 0.1 mole),加完后在115-120°反应2-3小时.冷却,加入250 g. 1 : 1 的冰水,过滤,得深黄色固体,乙醇精制的浅黄色固体17 g. (63.4%).m.p. 114-118,(可以进行下一步投料).再用乙醇精致3次,得到白色固体,m.p. 119-12O




回复人:rareearth, (有机化学研究生) 时间:2006-04-20 20:33:24   编辑 6楼
已经打分了。


回复人:乙酸乙酯,▲▲▲▲ (精细有机中间体) 时间:2006-04-21 09:56:14   编辑 7楼
rareearth
好人啊。


回复人:zhuyuqj, (现实就是生活) 时间:2006-04-21 22:34:29   编辑 8楼
实验写的很详细,做化工基本应该看的懂才对


回复人:卧虎藏龙, (河南大学化学化工学院03级) 时间:2006-04-22 09:36:46   编辑 9楼
到网上可以进行翻译的,而且快捷准确!


得分人:tangyyer-1,readpen-1,xmn78-1,乙酸乙酯-1,


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