反应详情

2-Bromoethyl 3-[(2-acetylthiomethyl-3-phenylpropionyl)amino]benzoate (compound of Example 123) (0.63 g) and 3-pyridinecarboxamide (0.17 g) are dissolved in methanol (10 ml), and the mixture is refluxed overnight. Methanol is distilled off under reduced pressure, and the residue is dissolved in ethyl acetate, washed with water and dried over anhydrous magnesium sulfate. Ethyl acetate is distilled off under reduced pressure. The residue is purified by a medium pressure column chromatography with silica gel (eluant, chloroform). The fractions containing the desired compound are collected, and chloroform is distilled off under reduced pressure to give the title compound (0.3 g) as an oily substance. IR (film; cm-1): 1715, 1685, 1660 Mass spectrum (SIMS) [M+H]+ : m/z 402

1. temperaturethe mixture is refluxed overnight
2. distillationMethanol is distilled off under reduced pressure
3. dissolutionthe residue is dissolved in ethyl acetate
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationEthyl acetate is distilled off under reduced pressure
7. customThe residue is purified by a medium pressure column chromatography with silica gel (eluant, chloroform)
8. additionThe fractions containing the desired compound
9. customare collected
10. distillationchloroform is distilled off under reduced pressure