HRID1696455

反应详情

EQUATION

反应方程式

HRID 1696455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2′-Nitro-4′-(trifluoromethyl)-[1,1′-biphenyl]-3-acetic acid ethyl ester (107 mg, 0.30 mmol) in THF (6 mL) was treated with about 150 mg of Raney® nickel (50 wt % in H2O). The reaction was shaken on a Parr apparatus under 50 psi of H2. After 4.5 h, another 200 mg of Raney® nickel was added and the reaction was shaken an additional 2 h under 50 psi H2. The reaction mixture was filtered through Celite®, concentrated in vacuo and purified via column chromatography to afford 2′-amino-4′-(trifluoromethyl)-[1,1′-biphenyl]-3-acetic acid ethyl ester (58 mg, 59% yield). MS (ESI) m/z: 324.2 (M+H+).

WORKUP

后处理

  1. stirringthe reaction was shaken an additional 2 h under 50 psi H2
  2. filtrationThe reaction mixture was filtered through Celite®
  3. concentrationconcentrated in vacuo
  4. custompurified via column chromatography