反应详情

Treat a solution of 5-methyl-3-(2,4,6-trimethylphenyl)imidazolo[5,4-b]pyridin-7-ylamine (0.05 g, 1.9 mmol), and N,N-diisopropylethylamine, (0.04 mL, 0.21 mmol) in 1,2-dichloroethane (5 mL) with chloroacetyl chloride (0.017 mL, 0.21 mmol). Heat the solution to reflux for 3 h, cool to ambient temperature, and pour into an aqueous potassium carbonate solution. Extract the resulting mixture with CH2Cl2 and wash with saturated aq NaCl. Separate the organic layer, dry over Na2SO4, filter, and concentrate. Purify by preparative TLC (5% MeOH in CH2Cl2) to obtain the title compound as a yellow solid.

1. temperatureHeat the solution
2. temperatureto reflux for 3 h
3. extractionExtract the resulting mixture with CH2Cl2
4. washwash with saturated aq NaCl
5. customSeparate the organic layer
6. dry with materialdry over Na2SO4
7. filtrationfilter
8. concentrationconcentrate
9. customPurify by preparative TLC (5% MeOH in CH2Cl2)