HRID1274146

反应详情

EQUATION

反应方程式

HRID 1274146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Compound (51) (5 mmol) was added to a solution of 4-amino-2-chloro-6,7-dimethoxy quinazoline (0.96 g, 4 mmol) in isoamyl alcohol (10 mL) at 25° C. The mixture was then stirred at 120° C. for 12 h. After cooling to room temperature, the desired product was filtered and rinsed with acetone to give 1.62 g (96%) of the title compound: TLC (Rf =0.30; 10% CH3OH/CH2Cl2); 1H NMR (DMSO) δ 11.90 (br, 1H), 10.30 (br, 1H), 9.80 (br, 1H), 9.00 (br, 1H), 8.80 (br, 1H), 7.80 (s, 1H), 7.69 (d, 1H, J=2.0), 7.41 (s, 1H), 7.19 (s, 1H), 3.86 (s, 3H), 3.85 (s, 3H), 3.76 (s, 3H); HRMS (FAB) m/z 421.1152 (M+H)+ (C16H18N8O4Cl requires 421.1110); Anal. (C16H18N8O4Cl·1/4CH3OH) C, H, N.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe desired product was filtered
  3. washrinsed with acetone