HRID1818959

反应详情

EQUATION

反应方程式

HRID 1818959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of compound 70.1 (1.0 mmol), compound 16.1 (1.0 mmol) and DMAP (1.0 mmol) in DMSO (10 mL) is heated at 90° C. for 30 minutes. The reaction is cooled, and partitioned between EtOAC and 1.0 N NaOH. The organic layer is separated, washed with brine, dried and concentrated to give a residue that was purified by preparative TLC (6% MeOH in dichloromethane) to provide 1-[3-(2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-5-fluoro-phenyl]-3-{5-[2-(thieno[3,2-d]pyrimidin-4-ylamino)-ethyl]-thiazol-2-yl}-urea (compound 70.2).

WORKUP

后处理

  1. temperatureThe reaction is cooled
  2. custompartitioned between EtOAC and 1.0 N NaOH
  3. customThe organic layer is separated
  4. washwashed with brine
  5. customdried
  6. concentrationconcentrated
  7. customto give a residue that
  8. customwas purified by preparative TLC (6% MeOH in dichloromethane)