反应详情

To a solution of the product of example 314 (800 mg) in acetic acid (20 ml) were added urea (2 g) and trimethylsilyl chloride (0.24 ml) at room temperature, and the mixture stirred for 2 hours. Sodium borohydride was added to the reaction mixture at room temperature, and the mixture was stirred for 1 hour. The solvent was distilled off under reduced pressure, and, chloroform, 2-propanol and water were added. The organic layer was extracted, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography eluting with chloroform-methanol-ammonium hydroxide (100:10:1) to give the titled compound (250 mg).

1. stirringthe mixture was stirred for 1 hour
2. distillationThe solvent was distilled off under reduced pressure, and, chloroform, 2-propanol and water
3. additionwere added
4. extractionThe organic layer was extracted
5. distillationthe solvent was distilled off under reduced pressure
6. customThe residue was purified by silica gel chromatography
7. washeluting with chloroform-methanol-ammonium hydroxide (100:10:1)