反应详情

温度

80 °C

A stirred solution of 1-benzhydryl-3-(tert-butyl-diphenyl-silanyloxy)-azetidine (162a) (4.0 g, 8.4 mmol) in DCE (60 ml) at room temperature is treated with 1-chloroethylchloroformate (1.2 ml, 10.9 mmol) and the reaction mixture is heated to 80° C. After 2 hours, the solvent is removed in vacuo and the residue is dissolved in methanol (60 ml) and heated to reflux. After 1 h the reaction mixture is poured into water (250 ml), acidified with hydrochloric acid (1M solution) and washed with EtOAc (3×75 ml). The aqueous solution is basified with saturated sodium bicarbonate solution and extracted with EtOAc (3×75 ml). The combined organic layers are washed with water (2×50 ml), brine (50 ml), dried over MgSO4. The solvent is removed in vacuo to yield the titled compound.

1. customthe solvent is removed in vacuo
2. dissolutionthe residue is dissolved in methanol (60 ml)
3. temperatureheated to reflux
4. additionAfter 1 h the reaction mixture is poured into water (250 ml)
5. washwashed with EtOAc (3×75 ml)
6. extractionextracted with EtOAc (3×75 ml)
7. washThe combined organic layers are washed with water (2×50 ml), brine (50 ml)
8. dry with materialdried over MgSO4
9. customThe solvent is removed in vacuo