HRID1785129

反应详情

EQUATION

反应方程式

HRID 1785129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This was prepared using the method described in example 4 using 4-chloro-6,7-dimethoxyquinazoline (160 mg, 0.71 mmol), N′-[3-(7-amino-6-chloro-1,3-benzodioxol-4-yl)prop-2-yn-1-yl]-N,N-dimethylurea (232 mg, 0.78 mmol) and sodium bis(trimethylsilyl)amide (1.0M in THF, 1.5 ml) in DMF (3 ml). The crude product was purified by column chromatography on silica using increasing concentrations of methanol in dichloromethane as eluent. There was thus obtained the title compound (265 mg, 77%) as a pale brown solid; NMR Spectrum:DMSOd6) 2.81 (s, 6H), 3.91 (s, 3H), 3.92 (s, 3H), 4.09 (d, 2H), 6.14 (s, 2H), 6.82 (t, 1H), 7.07 (s, 1H), 7.18 (s, 1H), 7.82 (s, 1H), 8.33 (s, 1H), 9.47 (s, 1H); Mass Spectrum: M+H+ 484/486.

WORKUP

后处理

  1. customThis was prepared
  2. customThe crude product was purified by column chromatography on silica using
  3. temperatureincreasing concentrations of methanol in dichloromethane as eluent