反应详情

温度

50 °C

A 0.5 M solution of zinc chloride in tetrahydrofuran (5.20 mL) is added dropwise at room temperature to a mixture of N-hydroxy-isobutyramidine (266 mg) and N-(1-cyano-piperidin-4-yl)-N-cyclopropyl-4-oxazol-5-yl-benzamide (600 mg) in ethyl acetate (25 mL). The reaction mixture is stirred at 50° C. for 3 h and cooled to room temperature. The precipitate is filtered off and heated to 100° C. for 2 h in a mixture of ethanol (10 mL) and glacial acetic acid (5 mL). The solvents are evaporated and the residue is chromatographed on silica gel [ethyl acetate/cyclohexane/methanol 9:9:2] to give the title compound. LC (method 6): tR=1.66 min; Mass spectrum (ESI+): m/z=422 [M+H]+.

1. temperaturecooled to room temperature
2. filtrationThe precipitate is filtered off
3. temperatureheated to 100° C. for 2 h in a mixture of ethanol (10 mL) and glacial acetic acid (5 mL)
4. customThe solvents are evaporated
5. customthe residue is chromatographed on silica gel [ethyl acetate/cyclohexane/methanol 9:9:2]