反应详情

温度

6 °C

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 6° 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.

1. temperaturecooled to 50 C
2. customquenched with 60 ml water
3. temperaturecooled to 5 C
4. filtrationThe solid was filtered
5. washwashed with water
6. customrecrystallized
7. dissolutionby dissolving in 50 ml hot acetonitrile
8. additionadding 10 ml of water
9. temperatureAfter cooling to 5 C
10. filtrationthe product was filtered
11. washwashed
12. customdried