反应 #570289

反应方程式

trichloroacetyl isocyanate

trichloroacetyl isocyanate

2-diphenylmethoxycarbonyl-3-oxothiomorpholine

bistrimethylsilyltrifluoroacetamide

→

2-diphenylmethoxycarbonyl-4-carbamoyl-3-oxothiomorpholine

收率 89.6%

溶剂

dichloromethane

反应条件

后处理

1. 1
   浓缩the mixture is concentrated
2. 2
   洗涤Fractions eluted with dichloromethane
3. 3
   workup.ADDITIONa mixture of dichloromethane and ethyl acetate (9:1)
4. 4
   浓缩concentrated

实验过程

To a mixture of 2-diphenylmethoxycarbonyl-3-oxothiomorpholine (327 mg, 1 mM), dichloromethane (8 ml), and bistrimethylsilyltrifluoroacetamide (0.53 ml). After 30 minutes' stirring from addition of trichloroacetyl isocyanate (0.18 ml), another trichloroacetyl isocyanate (0.06 ml) is added. After another 30 minutes' stirring, the mixture is concentrated and subjected to silica gel chromatography. Fractions eluted with dichloromethane and a mixture of dichloromethane and ethyl acetate (9:1) are combined and concentrated to give 2-diphenylmethoxycarbonyl-4-carbamoyl-3-oxothiomorpholine (332 mg). Yield 89.6%.

来源