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afmin

铁杆木虫 (小有名气)

[交流] 【求助】硫酰氯苯环氯化

各位大虾,请问高手,是否有人知道用硫酰氯作氯化剂进行苯环氯化
请站内消息联系我,谢谢!!!

[ Last edited by mooncakexzj on 2009-3-29 at 15:50 ]
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xqj666666

铁杆木虫 (小有名气)

如果有人知道请通知我
4楼2009-03-31 11:53:11
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afmin

铁杆木虫 (小有名气)

怎么没人回答的啊?郁闷中~~~
3楼2009-03-29 15:38:54
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TJFWAL

金虫 (著名写手)

小木虫之山野散人


nealu(金币+1,VIP+0):谢谢应助! 3-31 15:28
在OS上有一片文章,你可以看看.
对羟基苯甲酸乙酯的氯化.

Ethyl 3,5-dichloro-4-hydroxybenzoate. A tared 2-l. round-bottomed flask is equipped with an
efficient reflux condenser connected through a calcium chloride drying tube to a gas-absorption trap,
and is set up on a steam bath in a hood. In the flask are placed 250 g. (1.5 moles) of ethyl 4-
hydroxybenzoate (Note 1) and 444 g. (266 ml., 3.3 moles) of sulfuryl chloride. The mixture is warmed
on the steam bath (gently at first) until gas is no longer evolved (about 1 hour). Then 50 ml. of sulfuryl
chloride is added to the reaction flask, and the warming is continued until gas is no longer evolved. This
entire chlorination procedure requires about 1.5 hours. The excess sulfuryl chloride is then removed by
attaching a water pump through an empty safety flask to the reaction flask and warming on the steam
bath until no evidence of vapor can be detected above the white solid in the reaction flask. The residue
in the flask should weigh about 350 g. (Note 2). Recrystallization from a mixture of 600 ml. of ethanol
and 140 ml. of water gives 315–334 g. (83–88%) of ethyl 3,5-dichloro-4-hydroxybenzoate hydrate
(Note 3) melting at 110–114° with decomposition.




http://www.orgsyn.org/orgsyn/pdfs/CV3P0267.pdf

[ Last edited by TJFWAL on 2009-3-30 at 19:01 ]
人啊人............................
5楼2009-03-31 15:00:30
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afmin

铁杆木虫 (小有名气)

谢谢楼上的,有所启发!可惜我没钱哦!就不给你奖励了哦!不好意思
6楼2009-03-31 15:18:16
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