HRID1986193

反应详情

EQUATION

反应方程式

HRID 1986193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(2-{2-[3-(4-Methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophen-6-ylmethyl)-carbamic acid tert-butyl ester (1.36 g, 2.74 mmol) is dissolved in dichloromethane (20 mL) and TFA (3.2 mL) is added. After stirring for 20 hours, methanol is added and the mixture is passed through an SCX column. After eluting with methanol to remove the salts, 20% 2.0 M NH3/MeOH)/EtOAC is used to elute the product which is then passed through a 15 g silica gel column using the same solvent system. The title compound is obtained as a yellow solid (0.73 g, 68% yield). ES+(m/z) 397 [M+H].

WORKUP

后处理

  1. washAfter eluting with methanol
  2. customto remove the salts, 20% 2.0 M NH3/MeOH)/EtOAC
  3. washto elute the product which