反应详情

To a solution of trans-4-[(tert-butoxycarbonyl)(methyl)amino]cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 4; 8.1 g, 0.01 mol) in dioxane (13.5 mL) was added hydrogen chloride 4M in dioxane (27 mL). The mixture was stirred at room temperature for 24 hours. The precipitate obtained was filtrated and washed with ether. The crude was dissolved in water and potassium carbonate was added until pH=8-9. The product was extracted with ethyl acetate and the organic layer was washed with brine, dried and evaporated to dryness giving the title compound as a white solid (78%).

1. customThe precipitate obtained
2. filtrationwas filtrated
3. washwashed with ether
4. dissolutionThe crude was dissolved in water
5. additionpotassium carbonate was added until pH=8-9
6. extractionThe product was extracted with ethyl acetate
7. washthe organic layer was washed with brine
8. customdried
9. customevaporated to dryness