反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 45 °C
PROCEDURE
实验过程
A solution of the amine of Example 13 (0.873 g, 2.70 mmol) and tert-butyl{4-[(2S)oxiranylmethoxy]phenoxy}diphenylsilane (0.980 g, 2.42 mmol) in a mixture of methanol (20 mL) and THF (3 mL) was heated to 45° C. for 23 h. TLC shows characteristic product spot at Rf=0.25(silica gel plate; dichloromethane/chloroform/methanol: 20/5/2). The reaction mixture was cooled, silica gel (5 g) was added and the methanol was remove in vacuo. The reaction mixture, preabsorbed onto silica gel was applied to the top of a flash chromatography column (silica gel; dichloromethane/chloroform/methanol: 12/3/1) and purified in the standard manner. This procedure afforded 0.660 g of the title compound as a white foam.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- additionsilica gel (5 g) was added
- customthe methanol was remove in vacuo
- customThe reaction mixture, preabsorbed onto silica gel
- custompurified in the standard manner