HRID1051431

反应详情

EQUATION

反应方程式

HRID 1051431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

N-(4-bromothiazol-5-yl)acetamide from example 1.5 (1 g, 4.52 mmol), CuI(869 mg, 4.52 mmol) and Cs2CO3 (2.9 g, 9.1 mmol) were combined in a flask (backfilled with N2). Trans-N,N′-dimethylcyclohexane-1,2-diamine (630 mg, 4.52 mmol) and 4-methyl-1H-imidazole (446 mg, 5.4 mmol) in DMF (10 mL) were added and the mixture was stirred at 90° C. overnight. After the mixture was cooled to room temperature, the mixture was filtered through a syringe filter (washed with DMF). The filtrate purified by prep-HPLC to give 200 mg of the pure title compound (yield: 20%).

WORKUP

后处理

  1. temperatureAfter the mixture was cooled to room temperature
  2. filtrationthe mixture was filtered through a syringe
  3. filtrationfilter
  4. wash(washed with DMF)
  5. customThe filtrate purified by prep-HPLC