HRID1649253
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
6-(1-Piperazinyl)carbostyril hydrobromide (2.0 g) was suspended in 20 ml of DMF. After adding 2.34 ml of triethylamine, a solution of 1.43 g of 3,4-methylenedioxybenzoyl chloride in 2 ml of DMF was added dropwise to the mixture. After completion of addition, the mixture was stirred at room temperature for 30 minutes and the reaction mixture was poured in a large amount of water. Crystals which formed were collected by filtration and dried. Then, the crystals were purified through silica gel column chromatography and recrystallized from chloroform-methanol to give 1.9 g of 6-[4-(3,4-methylenedioxybenzoyl)-1-piperazinyl]carbostyril, m.p. 266°-267° C. (decomp.), yellow powders.
WORKUP
后处理
- additionAfter completion of addition
- customCrystals which formed
- filtrationwere collected by filtration
- customdried
- customThen, the crystals were purified through silica gel column chromatography
- customrecrystallized from chloroform-methanol