反应详情

温度

110 °C

In 2 ml of concentrated hydrochloric acid was dissolved 350 mg (0.73 mmol) of the benzyl compound (140b) and the solution was stirred under heating at 110° C. for 3 hours. To this reaction mixture was added a saturated aqueous solution of NaHCO3 and the solvent was distilled off under reduced pressure. The residue was extracted with ethyl acetate and the extract was washed with water and dried. The solvent was then distilled off and the residue was purified by silica gel column chromatography (ethyl acetate) to provide 150 mg (yield 53%) of Compound I-153 as crystals. mp 181-182° C.

1. distillationthe solvent was distilled off under reduced pressure
2. extractionThe residue was extracted with ethyl acetate
3. washthe extract was washed with water
4. customdried
5. distillationThe solvent was then distilled off
6. customthe residue was purified by silica gel column chromatography (ethyl acetate)