HRID1006655

反应详情

EQUATION

反应方程式

HRID 1006655 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 solution of the compound of step (a) (310 mg, 0.44 mmol) in methylene chloride (5 ml) was cooled to 0° C. and then treated with bromotrimethylsilane (303 mg, 1.98 mmol) and pyridine (215 mg, 3.70 mmol). The resulting mixture was stirred at 0° C. for 3 hours and then quenched with water (1 ml) containing sodium hydroxide (115 mg, 2.87 mmol). A yellow precipitate was formed, which was isolated by filtration and then partitioned between dilute sulphuric acid and methylene chloride. The organic phase was washed with brine, dried (MgSO4) and the solvent evaporated to give the title compound as a pale yellow solid (80 mg, 35%).

WORKUP

后处理

  1. customquenched with water (1 ml)
  2. customA yellow precipitate was formed
  3. customwhich was isolated by filtration
  4. custompartitioned between dilute sulphuric acid and methylene chloride
  5. washThe organic phase was washed with brine
  6. dry with materialdried (MgSO4)
  7. customthe solvent evaporated