反应详情

To a stirring slurry of 5-amino-4,6-dichloropyrimidine (3 g, 18.29 mmol) and indoline (2.057 mL, 18.29 mmol) in ethanol (7 mL) and water (43 mL) was added concentrated aqueous HCl (600 μL) and the mixture was refluxed for 3 h and left to stir at room temperature overnight. The reaction mixture was extracted with ethyl acetate, washed with water, brine, dried over MgSO4 and solvent evaporated. The resulting residue was triturated in 25% ethyl acetate in hexanes for 1 h then filtered to afford title compound 105 (1.55 g, 34%) as a tan solid. LRMS (ESI): (calc) 246.07. (found) 247.2 (MH)+.

1. temperaturethe mixture was refluxed for 3 h
2. waitleft
3. extractionThe reaction mixture was extracted with ethyl acetate
4. washwashed with water, brine
5. dry with materialdried over MgSO4 and solvent
6. customevaporated
7. customThe resulting residue was triturated in 25% ethyl acetate in hexanes for 1 h
8. filtrationthen filtered