反应详情

温度

80 °C

Add (5-tert-butyl-2-p-tolyl-2H-pyrazol-3-yl)-carbamic acid, 2,2,2-trichloro-ethyl ester (Preparation 38, 0.32 mmol, 0.1 r) over a solution of 1-[4-(5-amino-4-methyl-pyridin-2-yl)-piperazin-1-yl]-2,2-dimethyl-propan-1-one (0.3 mmol, 0.08 g) and potassium carbonate (0.3 mmol, 0.05 g) in acetonitrile (3 mL), and stir the solution for 4 hours at 80° C. Add water and extract with CH2Cl2. Combine the organic layers and wash with saturated aq. sodium chloride. Dry over sodium sulfate, filter, and concentrate under reduced pressure to give a residue. Subject residue to silica gel chromatography eluting with hexanes/ethyl acetate in gradient (from 20% to 80%). MS(ES+): m/z=532 [M+H].

1. extractionAdd water and extract with CH2Cl2
2. washwash with saturated aq. sodium chloride
3. dry with materialDry over sodium sulfate
4. filtrationfilter
5. concentrationconcentrate under reduced pressure
6. customto give a residue
7. washSubject residue to silica gel chromatography eluting with hexanes/ethyl acetate in gradient (from 20% to 80%)