反应详情

温度

120 °C

A suspension of N′-(6-tert-butyl-3-cyano-pyridin-2-yl)-N,N-dimethyl-formamidine (0.46 g, 2.0 mmol) and 3-amino-4-(4-tert-butoxycarbonylamino-phenylsulfanyl)-benzoic acid methyl ester [prepared in Example 385C] (0.75 g, 2.0 mmol) in AcOH (10 mL) was heated at 120° C. for 30 minutes under N2. After cooling to room temperature, the reaction mixture was portioned between AcOEt and H2O, 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 (CH2Cl2/MeOH=98/2) to give the title compound as off-white powder (0.53 g, 47%).

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 (CH2Cl2/MeOH=98/2)