HRID1170473

反应详情

EQUATION

反应方程式

HRID 1170473 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10% Pd/C (12 mg) was added to a solution of 2-(2-imidazol-1-yl-6-methyl-pyrimidin-4-yl)-pyrrolidine-1-carboxylic acid benzyl ester (112 mg, 0.308 mmol) and ethanol (3 mL) at rt. The reaction was vacuum purged with N2 then stirred under a balloon of H2 for 4 h. The reaction mixture was filtered through celite and concentrated. Column chromatography (10 g, DCM to 20% MeOH/DCM) afforded 63 mg (89%) of 2-imidazol-1-yl-4-methyl-6-pyrrolidin-2-yl-pyrimidine. [M+H]+ 230.16; 1H-NMR (400 MHz, CD3OD) δ 8.74 (s, 1H), 8.05 (s, 1H), 7.31 (s, 1H), 7.14 (s, 1H), 4.95 (s, 2H), 4.25 (t, 1H), 3.25 (m, 1H), 3.05 (m, 1H), 2.59 (s, 3H), 2.35 (m, 1H), 1.90 (m, 2H); 13C-NMR (100 MHz, CD3OD) δ 173.4, 170.4, 153.9, 136.0, 128.9, 116.8, 116.0, 62.1, 46.5, 32.7, 25.3, 22.7.

WORKUP

后处理

  1. custompurged with N2
  2. filtrationThe reaction mixture was filtered through celite and
  3. concentrationconcentrated