HRID1006655
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
- 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
- customquenched with water (1 ml)
- customA yellow precipitate was formed
- customwhich was isolated by filtration
- custompartitioned between dilute sulphuric acid and methylene chloride
- washThe organic phase was washed with brine
- dry with materialdried (MgSO4)
- customthe solvent evaporated