反应详情

To a solution of 7-(2-fluoro-4-iodo-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid (2-vinyloxy-ethoxy)-amide (54 mg, 0.11 mmol) in IMS (3 mL) was added aqueous hydrochloric acid (0.5 mL, 1M, 0.5 mmol). The reaction was stirred at room temperature for 1 hour then concentrated in vacuo. The resultant residue was dissolved in ethyl acetate (10 mL), washed with aqueous saturated sodium bicarbonate solution (10 mL) and the aqueous fraction extracted twice with ethyl acetate (2×10 mL). The combined organic fractions were washed with brine, dried (MgSO4) and concentrated in vacuo. The product was triturated with MeOH/diethylether to yield the title compound as a light brown solid (20 mg, 39%). 1H NMR (d6-DMSO, 400 MHz) 11.32 (1H, s), 8.69 (1H, s), 7.98 (1H, s), 7.49 (1H, dd, J=11.0, 2.0 Hz), 7.40 (2H, s), 7.18-7.14 (1H, m), 6.74 (1H, s), 5.92 (1H, t, J=8.8 Hz), 4.65 (1H, t, J=5.6 Hz), 3.75 (2H, t, J=5.0 Hz), 3.46 (2H, q, J=5.0 Hz). LCMS (Method A): RT=8.14 min, M+H+=457.

1. concentrationthen concentrated in vacuo
2. dissolutionThe resultant residue was dissolved in ethyl acetate (10 mL)
3. washwashed with aqueous saturated sodium bicarbonate solution (10 mL)
4. extractionthe aqueous fraction extracted twice with ethyl acetate (2×10 mL)
5. washThe combined organic fractions were washed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo
8. customThe product was triturated with MeOH/diethylether