HRID547564

反应详情

EQUATION

反应方程式

HRID 547564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

To a mixture of 4-aminoacetanilide 14 (3.55 g, 23.64 mmol) and 2-amino-4-chloro-6-methylpyrimidine 15 (3.73 g, 26 mmol) in ethanol (50 mL) was added. C.HCl (2 drops). The reaction mixture was stirred under reflux conditions for 2 h, cooled to 20° C. and the product was filtered washed with more ethanol and dried to give essentially pure 16 (6.38 g, 92%); mp (EtOH) 203-207° C.; 1H NMR [(CD3)2SO] δ 12.60 (br, 1 H, N+H), 10.50 (br 1 H, NH), 10.02 (s, 1 H, NH), 7.60-7.58 (br m, 6 H, NH2 & ArH), 6.13 (s, 1 H, H-5″), 2.26 (s, 3 H, CH3), 2.04 (s, 3 H, CH3); HRMS (FAB+), calc. for C13H16N5O (M+1) m/z 258.1355, found 258.1346.

WORKUP

后处理

  1. additionwas added
  2. filtrationthe product was filtered
  3. washwashed with more ethanol
  4. customdried