三光氣后續(xù)處理
各位大佬,我想用三光氣和雙羥基反應(yīng)生成氯甲酸酯。下面是查到的文獻(xiàn),請(qǐng)問(wèn)三光氣是怎樣被除掉的?
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.
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文獻(xiàn)中沒(méi)有提及到后處理,三光氣一般用堿液滴加低溫處理,注意通風(fēng)和防護(hù)。
具體可咨詢(xún)生產(chǎn)廠家。
堿液加入或者相反都需要控溫,反應(yīng)放熱的。然后萃取。
是利用氮?dú)饧訅簩⒎磻?yīng)液壓入液堿中進(jìn)行反應(yīng)吧
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