HRID1803866

反应详情

EQUATION

反应方程式

HRID 1803866 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

In a cylindrical quartz tube were placed 4-fluoro-2-methyl-benzoic acid methyl ester (1.2 g, 7.14 mmol), N-methylpiperazine (0.95 ml, 8.5 mmol), K2CO3 (990 mg, 7.14 mmol) and DMSO (4 ml). The reaction was heated for 20 hours at 110° C. until HPLC revealed the disappearance of the starting-material. DCM (15 ml) was added and the solution was washed twice with water and the organic phase was dried over anhydrous Na2SO4. The crude was purified by flash chromatography (DCM/MeOH 95:5) affording the desired compound (670 mg, 38%).

WORKUP

后处理

  1. customIn a cylindrical quartz tube were placed
  2. washthe solution was washed twice with water
  3. dry with materialthe organic phase was dried over anhydrous Na2SO4
  4. customThe crude was purified by flash chromatography (DCM/MeOH 95:5)