HRID1267516

反应详情

EQUATION

反应方程式

HRID 1267516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 950 mg (1.81 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-(2′-methyl-4-nitro-biphenyl-2-yl)-isobutyramide in 12 ml tetrahydrofuran and 3 ml water 608 mg (10.87 mmol) iron powder and 3 drops trifluoroacetic acid were added. After heating at 85° for 3 hrs., the reaction mixture was cooled to room temperature and evaporated. The residue was purified by chromatography (SiO2, hexane/ethyl acetate 1:4) to give 890 mg (99%) N-(4-amino-2′-methyl-biphenyl-2-yl)-2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-isobutyramide as pale yellow crystals, MS (ISP): 495.2 (M+H)+.

WORKUP

后处理

  1. temperatureAfter heating at 85° for 3 hrs
  2. customevaporated
  3. customThe residue was purified by chromatography (SiO2, hexane/ethyl acetate 1:4)