反应详情

To a stirred solution of N-(2,5-dimethyl-pyrazolo[1,5-a]pyrimidin-7-yl)-ethane-1,2-diamine (3.2 g, 16 mmol) and cyclopentanone (2.7 mL, 30 mmol) in methanol (30 mL)/acetic acid (3 mL) was added sodium cyanoborohydride (0.94 g, 15 mmol), portionwise. After stirring 1 hour the reaction was concentrated under reduced pressure and then extracted from saturated aqueous sodium bicarbonate with ethyl acetate. The combined extracts were dried (Na2SO4), concentrated under reduced pressure to give the crude product as a brown oil (5.6 g): +APcI MS (M+1)+ 274; 1H NMR (CDCl3) δ: 6.11 (s, 1H), 6.76 (s, 1H), 3.21 (t, 2H), 3.21 (m, 1H ), 3.04 (t, 1H), 2.42 (s, 3H), 2.40 (s, 3H).

1. concentrationwas concentrated under reduced pressure
2. extractionextracted from saturated aqueous sodium bicarbonate with ethyl acetate
3. dry with materialThe combined extracts were dried (Na2SO4)
4. concentrationconcentrated under reduced pressure