HRID1926472
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
To a flask were added 2.0 g 2-mercapto-5-methylbenzimidazole, 4.2 g potassium carbonate, 30 ml N,N-dimethylformamide and 3.9 g benzyl chloride. The reaction mixture was heated to 60 C for 16 hours, then cooled to 50 C and quenched with 60 ml water and cooled to 5 C. The solid was filtered and washed with water and then recrystallized by dissolving in 50 ml hot acetonitrile and adding 10 ml of water. After cooling to 5 C, the product was filtered, washed and dried resulting in 3.5 g white solid as a mixture of the 5-methyl and 6-methyl isomers.
WORKUP
后处理
- temperatureThe reaction mixture was heated to 60 C for 16 hours
- temperaturecooled to 50 C
- customquenched with 60 ml water
- temperaturecooled to 5 C
- filtrationThe solid was filtered
- washwashed with water
- customrecrystallized
- dissolutionby dissolving in 50 ml hot acetonitrile
- additionadding 10 ml of water
- temperatureAfter cooling to 5 C
- filtrationthe product was filtered
- washwashed
- customdried