HRID1157588

反应详情

EQUATION

反应方程式

HRID 1157588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 2,2,2-trifluoro-N-[2-(methylsulfonyl)ethyl]-N-[(3-nitrophenyl)methyl]acetamide (0.88 g, 2.5 mmol) in i-PrOH was added 10% Pd/C (80 mg, 0.08 mmol). A balloon filled with hydrogen gas was installed, and the reaction was stirred vigorously at rt. After 64 h, the reaction mixture was filtered through celite, adsorbed onto silica gel, and purified by column chromatography to generate the title compound in 93% yield. 1H NMR (400 MHz, CDCl3) δ 7.17 (t, J=7.5 Hz, 1H), 6.60-6.67 (m, 2H), 6.53 (s, 1H), 4.62 (s, 2H), 3.73 (t, J=6.9 Hz, 2H), 3.18 (t, J=6.8 Hz, 2H), 2.92 (s, 3H). ES-LC/MS m/z=324 [M+H]+.

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered through celite
  2. custompurified by column chromatography