HRID427728

反应详情

EQUATION

反应方程式

HRID 427728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

(5-Methoxy-2-nitro4-trifluoromethylphenyl)acetonitrile (D7) (85 g, 0.327 mol) in ethanol/water (9:1, 1.6 l) and glacial acetic acid (16 ml) was hydrogenated over 10% palladium on carbon (50 g) at 50 psi for 0.5 h at room temperature. The reaction mixture was filtered and evaporated in vacuo. The residue was partitioned between aqueous K2CO3 (1 l) and dichloromethane (2×1 l) and the combined organic extract was dried (Na2SO4) and evaporated to afford the title indole (67.63 g, 96%) as a grey solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customevaporated in vacuo
  3. customThe residue was partitioned between aqueous K2CO3 (1 l) and dichloromethane (2×1 l)
  4. extractionthe combined organic extract
  5. dry with materialwas dried (Na2SO4)
  6. customevaporated