HRID582794
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
- 50 °C
PROCEDURE
实验过程
1.015 g of 2-amino-2-adamantanecarboxylic acid and 6 ml of bis(trimethylsilyl)acetamide in 10 ml of DCM is heated to reflux for one and a half hours. 0.75 ml of benzyloxycarbonyl chloride is added and the mixture is heated at 50° C. for 15 minutes. The reaction medium is cooled to -70° C., decomposition is then effected by adding ice and the mixture is extracted with AcOEt. The organic phase is washed with water (twice) and with brine, dried over MgSO4 and evaporated under vacuum. The product crystallizes in hexane; 1.164 g are obtained.
WORKUP
后处理
- temperatureto reflux for one and a half hours
- temperatureThe reaction medium is cooled to -70° C.
- additionby adding ice
- extractionthe mixture is extracted with AcOEt
- washThe organic phase is washed with water (twice) and with brine
- dry with materialdried over MgSO4
- customevaporated under vacuum
- customThe product crystallizes in hexane
- custom1.164 g are obtained