反应详情

温度

65 °C

To a solution of trans-4-[[3-({2-chloro-5-methoxy-4-[(E)-2-methoxyvinyl]phenyl}amino)-3-oxopropyl](methyl)amino]cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 122; 0.36 g, 0.17 mmol) in anhydride tetrahydrofurane (0.5 mL) was added dropwise hydrochloric acid 2M (0.34 mL, 0.7 mmol). The mixture was stirred at 65° C. for 5 hours and a half. A mixture of water/ice was poured into the reaction and then extracted with ethyl acetate. The organic layer was washed with water and brine, dried and the solvent was removed under reduced pressure. The crude obtained was purified by column chromatography with silica gel, eluting with methylen chloride/methanol (95:5) to give the title compound as an oil (90%).

1. additionwas poured into the reaction
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with water and brine
4. customdried
5. customthe solvent was removed under reduced pressure
6. customThe crude obtained
7. customwas purified by column chromatography with silica gel
8. washeluting with methylen chloride/methanol (95:5)