HRID1639802

反应详情

EQUATION

反应方程式

HRID 1639802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of a crudely purified product (6.00 g, purity 50%) of methyl 4-fluoro-2-methyl-3-nitrobenzoate and wet palladium carbon (10 wt %, 300 mg, 2.81 mmol) in methanol (100 mL) was stirred under hydrogen atmosphere for 4 hr. The catalyst was filtered off through celite, the filtrate was concentrated under reduced pressure, and the residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/20→1/10) to give the title compound (2.13 g, yield 42%).

WORKUP

后处理

  1. filtrationThe catalyst was filtered off through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customthe residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/20→1/10)