反应详情

Benzyl 3-[(2-acetylthiomethyl-3-phenylpropionyl)amino]benzoate (2.0 g) is dissolved in acetonitrile (20 ml), and thereto is added 28% aqueous ammonia (15 ml), and the mixture is stirred at room temperature for one hour. The reaction mixture is adjusted to pH 2.5 with 20% hydrochloric acid under ice cooling and is extracted with ethyl acetate (70 ml). The extract is washed with water, and ethyl acetate is distilled off under reduced pressure. The residue is purified by a medium pressure column chromatography with CHP-20P (eluant, water-acetonitrile). The fractions containing the desired compound are collected, and acetonitrile is distilled off under reduced pressure and the residue is extracted with ethyl acetate (100 ml). The extract is dried over anhydrous magnesium sulfate, and ethyl acetate is distilled off under reduced pressure to give the title compound (0.9 g) as a colorless oily substance.

1. extractionis extracted with ethyl acetate (70 ml)
2. washThe extract is washed with water, and ethyl acetate
3. distillationis distilled off under reduced pressure
4. customThe residue is purified by a medium pressure column chromatography with CHP-20P (eluant, water-acetonitrile)
5. additionThe fractions containing the desired compound
6. customare collected
7. distillationacetonitrile is distilled off under reduced pressure
8. extractionthe residue is extracted with ethyl acetate (100 ml)
9. dry with materialThe extract is dried over anhydrous magnesium sulfate, and ethyl acetate
10. distillationis distilled off under reduced pressure