HRID1785144

反应详情

EQUATION

反应方程式

HRID 1785144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This was prepared by the method described in example 4 but using 1-{3-[(4-chloro-6-methoxyquinazolin-7-yl)oxy]propyl}-4-methylpiperazin-2-one (140 mg, 0.38 mmol), 5-chloro-7-(4-methoxybut-1-yn-1-yl)-1,3-benzodioxol-4-amine (107 mg, 0.42 mmol) and sodium bis(trimethylsilyl)amide (1.0M in THF, 0.81 ml) in DMF (2 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 (150 mg, 67%) as a pale orange solid; NMR Spectrum:(DMSOd6) 2.04 (quintet, 2H), 2.20 (s, 3H), 2.59 (t, 2H), 2.72 (t, 2H), 2.91 (s, 2H), 3.30 (s, 3H), 3.32 (t, 2H), 3.47 (t, 2H), 3.53 (t, 2H), 3.94 (s, 3H), 4.14 (t, 2H), 6.14 (s, 2H), 7.07 (s, 1H), 7.15 (s, 1H), 7.83 (s, 1H), 8.32 (s, 1H), 9.49 (s, 1H);

WORKUP

后处理

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