反应详情

To a solution containing 1-formyl-4-(2-hydroxyethyl)piperazine (1.90 g, 12 mmol), 2-mercaptobenzimidazole (1.50 g, 10 mmol), and N,N-diisopropylethylamine (1.80 g, 14 mmol) in propionitrile (16 mL), cyanomethyltrimethylphosphonium iodide (2.80 g, 11.5 mmol) was added under argon, and the mixture was refluxed for 2 hours. After cooling, the reaction mixture was poured into water (100 mL), and the liquid was subjected to extraction with chloroform (100 mL×3) . The organic layer was washed with saturated brine, followed by drying over sodium sulfate anhydrate and removing the solvent through filtration. The thus-formed crude product was crystallized from acetone-diethyl ether, thereby yielding 2.50 g of 1-formyl-4-[2-(benzimidazol-2-ylthio)ethyl]piperazine (yield: 86%) as a colorless crystalline powder.

1. additionwas added under argon
2. temperaturethe mixture was refluxed for 2 hours
3. temperatureAfter cooling
4. extractionthe liquid was subjected to extraction with chloroform (100 mL×3)
5. washThe organic layer was washed with saturated brine
6. dry with materialby drying over sodium sulfate anhydrate
7. customremoving the solvent
8. filtrationthrough filtration
9. customThe thus-formed crude product
10. customwas crystallized from acetone-diethyl ether