HRID582794

反应详情

EQUATION

反应方程式

HRID 582794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto reflux for one and a half hours
  2. temperatureThe reaction medium is cooled to -70° C.
  3. additionby adding ice
  4. extractionthe mixture is extracted with AcOEt
  5. washThe organic phase is washed with water (twice) and with brine
  6. dry with materialdried over MgSO4
  7. customevaporated under vacuum
  8. customThe product crystallizes in hexane
  9. custom1.164 g are obtained