HRID1157585

反应详情

EQUATION

反应方程式

HRID 1157585 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 N-[2-(dimethylamino)ethyl]-2,2,2-trifluoro-N-[(3-nitrophenyl)methyl]acetamide (204 mg, 0.64 mmol) in i-PrOH was added 10% Pd/C (20 mg, 0.02 mmol). A balloon charged with H2 was installed, and the reaction was stirred at rt under a hydrogen atmosphere. After 17 h, the reaction mixture was filtered through celite and adsorbed onto silica gel. The crude product was purified by column chromatography to generate the title compound in 62% yield. 1H NMR (400 MHz, CDCl3) δ 7.10 (t, J=7.9 Hz, 1H), 6.69-6.70 (m, 2H), 6.58 (d, J=7.9 Hz, 1H), 3.76 (s, 2H), 2.75 (t, J=6.0 Hz, 2H), 2.49 (t, J=6.0 Hz, 2H), 2.24 (s, 6H). ES-LC/MS m/z=290 [M+H]+.

WORKUP

后处理

  1. additionA balloon charged with H2
  2. filtrationthe reaction mixture was filtered through celite
  3. customThe crude product was purified by column chromatography