反应详情

841 g of 6-acetyl-2-(2-bromopropionylamino)-3-(2-chlorobenzoyl)-4,5,6,7-tetrahydro-thieno[2,3 -C]pyridine was dissolved in a 0.72 liters of dichloroethane and 1.08 liters of ethyl acetate, into which ammonia gas was introduced at -10° C. The mixture was subjected to reaction in an autoclave at 100° C. for 1 hour. After completion of the reaction, excess ammonia gas was removed and the reaction solution was poured into 3N HCl under ice-cooling conditions. After extraction with ethyl acetate, the aqueous phase was neutralized with a saturated sodium carbonate aqueous solution, followed by repeating extraction with chloroform. The resultant organic phase was washed with a saturated saline solution, followed by drying with anhydrous magnesium sulfate and removal of the solvent by distillation under reduced pressure to obtain 636.8 g of the intended compound.

1. additionwas introduced at -10° C
2. customThe mixture was subjected to reaction in an autoclave at 100° C. for 1 hour
3. customwas removed
4. additionthe reaction solution was poured into 3N HCl under ice-
5. temperaturecooling conditions
6. extractionAfter extraction with ethyl acetate
7. extractionextraction with chloroform
8. washThe resultant organic phase was washed with a saturated saline solution
9. dry with materialby drying with anhydrous magnesium sulfate and removal of the solvent by distillation under reduced pressure