HRID358494

反应详情

EQUATION

反应方程式

HRID 358494 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.5 Grams of 6-(1-piperazinylcarbonyl)-3,4-dihydrocarbostyril and 1.5 g of triethylamine were suspended in 10 ml of dichloromethane. Under ice-cooled and stirring condition, 1.4 g of p-toluenesulfonylchloride in 10 ml of dichloromethane solution was added dropwise to the suspension and the reaction was continued for additionally 3 hours at a room temperature, further continued for 1 hour under ice-cooled condition. The crystals formed in the reaction mixture were collected by filtration and recrystallized from chloroform-ether to obtain 1.4 g of 6-[4-(p-toluenesulfonyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril. Colorless granular crystals. Melting point: 280°-282° C.

WORKUP

后处理

  1. temperatureUnder ice-cooled
  2. additionwas added dropwise to the suspension
  3. waitfurther continued for 1 hour under ice-
  4. temperaturecooled condition
  5. customThe crystals formed in the reaction mixture
  6. filtrationwere collected by filtration
  7. customrecrystallized from chloroform-ether