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三光气后续处理

作者 皛槑zxm
来源: 小木虫 150 3 举报帖子
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各位大佬,我想用三光气和双羟基反应生成氯甲酸酯。下面是查到的文献,请问三光气是怎样被除掉的?
Homobifunctional crosslinker 2 was prepared bymodification of a previously reportedmethod. 2,20-dithiodiethanol (16.7mmol) and triethylamine (34.7 mmol) were dissolved in 20 mL of dry CH2Cl2 and cooled to 0 1C under stirring. Next, triphosgene (11.7mmol) in 10 mL of CH2Cl2 was added dropwise. After being stirred for 1 h, the reaction mixture was poured into 150 mL of ether to cease the reaction. Then, the mixture was filtered and concentrated under vacuum. The residue was dissolved in 5 mL of CH2Cl2 followed by addition of 50 mL of hexane and the target compound was obtained as yellow solid without further purification. 返回小木虫查看更多

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  • 中国加油

    文献中没有提及到后处理,三光气一般用碱液滴加低温处理,注意通风和防护。
    具体可咨询生产厂家。

  • 中国加油

    引用回帖:
    3楼: Originally posted by 皛槑zxm at 2020-09-09 15:12:06
    您好 请问是把碱液加入到反应后的烧瓶中,然后用有机溶剂萃取所要的产物吗?  我之前看到一篇说是用氮气将反应溶液吹到碱液中,请问具体操作是什么?...

    碱液加入或者相反都需要控温,反应放热的。然后萃取。
    是利用氮气加压将反应液压入液碱中进行反应吧

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