HRID1477566

反应详情

EQUATION

反应方程式

HRID 1477566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

An acetic acid (15 mL)-water (35 mL) mixed solution of 6-chloro-4-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazin-2(1H)-one (1.00 g, 3.23 mmol) synthesized in Reference Synthesis Example 2 and palladium hydroxide-activated carbon catalyst (100 mg) was stirred under hydrogen atmosphere at room temperature for 3 days. After completion of the reaction, the reaction solution was filtered with Celite and the filtered residue was washed with methanol, followed by concentrating the obtained solution under reduced pressure. Toluene was added to the residue and the mixture was azeotropically dehydrated four times. The obtained residue was dried under reduced pressure to obtain the title compound (876 mg, yield 99%).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationthe reaction solution was filtered with Celite
  3. washthe filtered residue was washed with methanol
  4. concentrationby concentrating the obtained solution under reduced pressure
  5. additionToluene was added to the residue
  6. customThe obtained residue was dried under reduced pressure