HRID352901

反应详情

EQUATION

反应方程式

HRID 352901 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a mixed solvent of benzene (10 ml) and methanol (10 ml), 1-[(6-chloronaphthalen-2-yl)sulfonyl]-4-[4-(pyridin-4-yl)benzoyl]piperazine (300 mg) obtained in Example A-1 was dissolved at room temperature, followed by the addition of methyl iodide (1 ml). To the resulting mixture, the same amount of methyl iodide was added three times at intervals of 24 hours, followed by heating under reflux for 4 days. The reaction mixture was distilled under reduced pressure and the residue was washed with methanol, collected by filtration and dried, whereby the title compound (229 mg, 58%) was obtained as a yellow solid.

WORKUP

后处理

  1. dissolutionwas dissolved at room temperature
  2. temperatureby heating
  3. temperatureunder reflux for 4 days
  4. distillationThe reaction mixture was distilled under reduced pressure
  5. washthe residue was washed with methanol
  6. filtrationcollected by filtration
  7. customdried