HRID1514329

反应详情

EQUATION

反应方程式

HRID 1514329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A mixture of 5-bromo-2-chloropyrimidin-4-yl-(5-cyclopropyl-1H-pyrazol-3-yl)-amine (313 mg, 1.00 mmol) and 4-dimethylaminobenzylamine (225 mg, 1.5 mmol) in 1-butanol (20 mL) was heated to 170° C. in a 50 mL sealed tube for 3 h. The mixture was cooled and diluted with ethyl acetate. The organic layer was washed with 2 N sodium hydroxide, water and brine and dried over sodium sulfate. The solution was concentrated, redissolved in DMF and purified by preparative reverse phase HPLC to give the desired product (124 mg, 29%) as a white solid.

WORKUP

后处理

  1. customsealed tube for 3 h
  2. temperatureThe mixture was cooled
  3. washThe organic layer was washed with 2 N sodium hydroxide, water and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationThe solution was concentrated
  6. dissolutionredissolved in DMF
  7. custompurified by preparative reverse phase HPLC