HRID1927529

反应详情

EQUATION

反应方程式

HRID 1927529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of Example 154c (0.59 g, 1.54 mmol) in DMF (60 ml) was subjected to hydrogenation using activated Raney-Ni (0.3 g) at 50 psi for 3 h. It was filtered through a bed of celite, concentrated and purified using flash chromatography (silica gel, methanol/chloroform) to obtain the title compound. Yield: 0.39 g, (71%); 1HNMR (DMSO-d6): δ 2.6 (s, 3H, CH3), 3.88 (s, 3H, CH3), 4.65 (q, 2H, CH2), 5.6 (s, 2H, NH2), 6.65 (s, 2H, Ar), 8.0 (s, 1H, Ar), 8.16 (s, 1H, Ar); MS: m/e EI+) 351 (M+).

WORKUP

后处理

  1. customfor 3 h
  2. filtrationIt was filtered through a bed of celite,
  3. concentrationconcentrated
  4. custompurified