反应详情

温度

80 °C

1H-indazole-4-carbonitrile (commercially available from Insight Chemical Solutions Ltd., 298 mg, 1.957 mmol) in dry N,N-Dimethylformamide (DMF) (1 ml), under nitrogen was treated with NaH (94 mg, 2.348 mmol). A solution of ethyl 3-bromo-2,2-dimethylpropanoate (D98) (450 mg, 2.153 mmol), in DMF (2 ml), was then added to the dark brown mixture. The reaction mixture was heated to 80° C. overnight then concentrated in vacuo. The residue was dissolved in EtOAc and the organic phase was washed with water then brine, dried and concentrated to give a brown gum. Purification of the residue by flash chromatography on silica gel [gradient ethyl acetate/cyclohexane] gave the title compound (217 mg, 86%) as a yellow oil. MS (ES) C15H15N3O2 requires 271, found 272 [M+H]+

1. concentrationthen concentrated in vacuo
2. dissolutionThe residue was dissolved in EtOAc
3. washthe organic phase was washed with water
4. dry with materialbrine, dried
5. concentrationconcentrated
6. customto give a brown gum
7. customPurification of the residue by flash chromatography on silica gel [gradient ethyl acetate/cyclohexane]