反应详情

22.7 G. (150 mmoles) of 2-benzyloxyethanol is added dropwise with stirring to 188 ml. (300 mmoles) of a 17.2% phosgene solution in benzene cooled in an ice bath with protection from moisture. The addition is complete in 40 minutes and the solution is stirred in the ice bath for an additional hour. The reaction mixture is allowed to warm to room temperature and stirred overnight. A stream of nitrogen is passed through the solution to remove the excess phosgene and HCl. The reaction mixture is evaporated to dryness in vacuo affording 32.2 g. of a light orange residual oil. Infrared analysis reveals a strong carbonyl absorption and minimal hydroxy absorption. The material is used as is in the next step.

1. additionThe addition
2. stirringstirred overnight
3. customto remove the excess phosgene and HCl
4. customThe reaction mixture is evaporated to dryness in vacuo
5. customaffording 32.2 g
6. customa strong carbonyl absorption and minimal hydroxy absorption