HRID216828

反应详情

EQUATION

反应方程式

HRID 216828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (8-chloro-2-(2-chlorophenyl)quinolin-3-yl)methanamine (144.8 mg, 0.478 mmol), 2-amino-6-chloropurine (89.1 mg, 0.525 mmol) and N,N-diisopropylethylamine, redestilled, 99.5% (0.166 mL, 0.955 mmol) in 1-butanol, anhydrous, 99.8% (5.24 mL) was heated to reflux and stirred overnight. The reaction was cooled solvents removed and subjected to chromatography, 89:9:1 (DCM/MeOH,NH4OH)gradient, 1H NMR (400 MHz, DMSO-d6) δ ppm 12.08 (1H, br. s.), 8.36 (1H, s), 8.01 (1H, d, J=8.2 Hz), 7.92 (1H, d, J=6.3 Hz), 7.47-7.71 (8H, m), 5.56 (2H, br. s.), 4.59 (2H, br. s.) Mass Spectrum (ESI) m/e=436.1 (M+1).

WORKUP

后处理

  1. temperatureto reflux
  2. temperatureThe reaction was cooled solvents
  3. customremoved