HRID709089
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
To a solution of 6-(benzylsulfanyl)-2,3-dimethoxypyridine (Intermediate 44, 0.2 g, 0.76 mmol) in dichloromethane (1 ml) was added a solution of boron tribromide in dichloromethane (1 M, 0.77 g, 3.1 mmol) at −5° C. and reaction was stirred for 1 hour at 0° C. The temperature was gradually allowed to rise to room temperature before the mixture was stirred for a further 1 hour at room temperature. Upon cooling to 0° C. water (10 ml) was added drop-wise and the resulting mixture was filtered and the solid was washed with water (2 ml) followed by ethyl acetate (5 ml) and dried under vacuum at 40° C. to yield 6-(benzylsulfanyl)-3-hydroxypyridin-2(1H)-one (35 mg, 20%).
WORKUP
后处理
- customreaction
- customto rise to room temperature before the mixture
- stirringwas stirred for a further 1 hour at room temperature
- additionwas added drop-wise
- filtrationthe resulting mixture was filtered
- washthe solid was washed with water (2 ml)
- customdried under vacuum at 40° C.