HRID1984884

反应详情

EQUATION

反应方程式

HRID 1984884 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of trans-{4-[(4-dimethylamino-quinazolin-2-ylamino)-methyl]-cyclohexylmethyl}-carbamic acid tert-butyl ester (20.1 g, 48.6 mmol) in EtOAc (200 mL) was added 4 M hydrogen chloride in EtOAc (200 mL). The mixture was stirred at ambient temperature for 90 min and concentrated to give a solid. The solid was alkalized with saturated aqueous NaHCO3 (pH=9), concentrated, and purified by flash chromatography (NH silica gel, 33% MeOH in CHCl3) to give trans-N2-(4-aminomethyl-cyclohexylmethyl)-N4,N4-dimethyl-quinazoline-2,4-diamine (14.7 g, 97%) as a white solid.

WORKUP

后处理

  1. concentrationconcentrated
  2. customto give a solid
  3. concentrationconcentrated
  4. custompurified by flash chromatography (NH silica gel, 33% MeOH in CHCl3)