HRID53504
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
8.06 g of N-phenylpyrrolidinone were dissolved in 33 ml glacial acetic acid; the mixture was cooled to 0°-5° C. and then a solution of 2.65 ml bromine in 12 ml of glacial acetic acid was added dropwise. Stirring was continued for 30 minutes at room temperature. Work-up was accomplished by pouring the mixture into 1 l of water and neutralizing the mixture with KOH. The solid was filtered and dissolved in ethylacetate and washed with a sodium thiosulphate solution until the brown colour disappeared; washing with brine and drying with MgSO4 provided 8.5 g of a white crystalline mass that could be recrystallized from ether; m.p. 102° C.
WORKUP
后处理
- temperaturethe mixture was cooled to 0°-5° C.
- filtrationThe solid was filtered
- dissolutiondissolved in ethylacetate
- washwashed with a sodium thiosulphate solution until the brown colour
- washwashing with brine
- dry with materialdrying with MgSO4
- customprovided 8.5 g of a white crystalline mass that
- customcould be recrystallized from ether