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