HRID351740

反应详情

EQUATION

反应方程式

HRID 351740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-bromo-5-(1-hydroxy-1-methylethyl)pyridine from Step 1 (3.1 mmol) in chloroform (10 mL) was added m-chloroperoxybenzoic acid 70% (1.5 eq) and the resulting mixture was stirred at room temperature for 18 hours. An excess of calcium hydroxide was added and after stirring for 5 minutes, the mixture was filtered through celite and the filtrate was evaporated. The crude material was chromatographed on silica gel eluting with 10% ethanol in methylene chloride (saturated with ammonia) to afford the 3-bromo-5-(1-hydroxy-1-methylethyl)pyridine-N-oxide compound as a solid.

WORKUP

后处理

  1. stirringafter stirring for 5 minutes
  2. filtrationthe mixture was filtered through celite
  3. customthe filtrate was evaporated
  4. customThe crude material was chromatographed on silica gel eluting with 10% ethanol in methylene chloride (saturated with ammonia)