HRID386169

反应详情

EQUATION

反应方程式

HRID 386169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

7-(8-Chloro-3-methyl-imidazo[1,5-a]pyrazin-1-yl)-2-phenyl-quinoline was dissolved in 10.0 mL of 2.0M NH3 in IPA and 5.0 mL of CH2Cl2. The reaction was heated to 110° C. for 64 h. The salts were filtered off and washed with CH2Cl2. Purified with silica gel column chromatography [Jones Flashmaster, 10 g cartridge, eluting with 1% MeOH:EtOAc] to yield a dark yellow solid; 1H NMR (400 MHz, CDCl3) δ 2.71 (s, 3H), 5.61 (brs, 2H), 7.13 (d, 1H, J=5.1 Hz), 7.2 (d, 1H, J=5.1 Hz), 7.48-7.56 (m, 3H), 7.89-7.97 (m, 3H), 8.18-8.21 (m, 2H), 8.27 (d, 1H, J=8.6 Hz), 8.39 (s, 1H); MS (ES+): 352.06 (M+1), 353.07 (M+2), 354.09 (M+3).

WORKUP

后处理

  1. filtrationThe salts were filtered off
  2. washwashed with CH2Cl2
  3. customPurified with silica gel column chromatography [Jones Flashmaster, 10 g cartridge, eluting with 1% MeOH:EtOAc]
  4. customto yield a dark yellow solid