반응 #1843615

반응 방정식

triethylamine

5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthol

trichloromethyl chloroformate

benzene

→

5,6,7,8-Tetrahydro-5,5,8,8-tetramethyl -2-naphthyl chloroformate

용매

water

반응 조건

후처리

1. 1
   추출the mixture is extracted with ethyl ether
2. 2
   기타the organic phase is separated after settling
3. 3
   건조dried over magnesium sulphate
4. 4
   기타evaporated
5. 5
   기타The residue obtained
6. 6
   기타is purified by chromatography on a silica column
7. 7
   세척eluted with a mixture of dichloromethane and hexane (40:60)
8. 8
   기타After evaporation of the solvents, 4 g (75%) of the expected chloroformate
9. 9
   기타are collected in the form of a colorless oil

실험 절차

4.1 g (20 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthol, 1.2 ml of trichloromethyl chloroformate and 40 ml of benzene are introduced into a round-bottomed flask. 3 ml (21 mmol) of triethylamine are added dropwise and the mixture is stirred at room temperature for twelve hours. The reaction medium is poured into water, the mixture is extracted with ethyl ether and the organic phase is separated after settling has taken place, then dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column and eluted with a mixture of dichloromethane and hexane (40:60). After evaporation of the solvents, 4 g (75%) of the expected chloroformate are collected in the form of a colorless oil.

출처