HRID324415

反应详情

EQUATION

反应方程式

HRID 324415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A stirred solution of the product from step (i) (0.60 g) in dichloromethane (15 ml) was treated with triethylsilane (0.225 ml) and cooled to 0° C. Boron trifluoride etherate (0.65 ml) was added in four equal portions at 5 minute intervals and the reaction stirred at room temperature for 16 hours. The reaction was poured into saturated sodium bicarbonate solution (200 ml) and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated to give a yellow solid which was purified by reverse phase chromatography eluting with 50% to 80% methanol in 0.1% aqueous ammonium acetate.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe extracts were dried (MgSO4)
  3. customevaporated
  4. customto give a yellow solid which
  5. customwas purified by reverse phase chromatography
  6. washeluting with 50% to 80% methanol in 0.1% aqueous ammonium acetate