反应详情

温度

120 °C

A suspension of N′-(3-cyano-6-isopropyl-pyridin-2-yl)-N,N-dimethyl-formamidine (2.00 g, 9.3 mmol) and 3-amino-4-(4-tert-butoxycarbonylamino-phenylsulfanyl)-benzoic acid methyl ester (3.46 g, 9.3 mmol) in AcOH (40 mL) was heated at 120° C. for 20 minutes under N2. After cooling to room temperature, the reaction mixture was portioned between AcOEt (150 mL) and H2O (200 mL), and then made basic to pH 9 with K2CO3 under stirring. The organic layer was separated, washed with 10% NaHCO3, H2O and brine, dried over MgSO4, and evaporated to give pale brown oil. The oily residue was separated by silica gel column chromatography (AcOEt/n-hexane=5/1) to give yellow crystal. Further purification by washing with cold AcOEt (15 mL) gave the title compound as slightly yellow crystal (3.27 g, 65%).

1. temperatureAfter cooling to room temperature
2. customThe organic layer was separated
3. washwashed with 10% NaHCO3, H2O and brine
4. dry with materialdried over MgSO4
5. customevaporated
6. customto give pale brown oil
7. customThe oily residue was separated by silica gel column chromatography (AcOEt/n-hexane=5/1)
8. customto give yellow crystal
9. customFurther purification
10. washby washing with cold AcOEt (15 mL)