HRID7497

反应详情

EQUATION

反应方程式

HRID 7497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

The starting material 5-benzyloxy-2-fluoro-4-methylnitrobenzene was obtained by adding benzyl bromide (3 ml, 25 mmol) to a solution of 2-fluoro-5-hydroxy-4-methylnitrobenzene (3.92 mg, 23 mmol) in DMF (70 ml) containing potassium carbonate (9.5 g, 68 mmol). After stirring for 3 hours at 60° C. the mixture was diluted with water and adjusted to pH2. After extraction with ethyl acetate, the organic layer was washed with water and then brine, dried (MgSO4) and the solvent evaporated. The solid was filtered off, washed with hexane and dried under vacuum to give 5-benzyloxy-2-fluoro-4-methylnitrobenzene (4.83 g, 80%).

WORKUP

后处理

  1. extractionAfter extraction with ethyl acetate
  2. washthe organic layer was washed with water
  3. dry with materialbrine, dried (MgSO4)
  4. customthe solvent evaporated
  5. filtrationThe solid was filtered off
  6. washwashed with hexane
  7. customdried under vacuum