反应详情

A sample (0.26 g, 0.49 mmol) of (3-{4-[3-Methyl-4-(pyridin-3-yloxy)-phenylamino]-pyrido[3,4-d]pyrimidin-6-yl}-3-aza-bicyclo[3.1.0]hex-6-yl)-carbamic acid tert-butyl ester was treated with 0.5 mL of trifluoroacetic acid and immediately concentrated in vacuo. The residue was dissolved in chloroform and washed with saturated sodium bicarbonate. The aqueous layer was back extracted several times with chloroform. The organics were dried over sodium sulfate and evaporated to afford 206 mg of the title compound. A pure sample was obtained by crystallization from methanol and isopropyl ether. 1H NMR (CDCl3): δ 8.96 (s, 1), 8.53 (s, 1), 8.33 (m, 2), 7.65 (m, 1), 7.55 (m, 1), 7.21 (m, 2), 6.96 (d, 1), 615 (s, 1), 3.76 (d, 2), 3.54 (m, 2), 2.26 (s, 3), 2.24 (m, 1), 1.76 (m, 2). M.S. (m+1): 426. HPLC retention time (minutes): 3.919.

1. concentrationimmediately concentrated in vacuo
2. dissolutionThe residue was dissolved in chloroform
3. washwashed with saturated sodium bicarbonate
4. dry with materialThe organics were dried over sodium sulfate
5. customevaporated