反应详情

1-[4-(4-amino-6-vinylpyrrolo[2,1-f][1,2,4]triazin-5-yl)phenyl]-3-[4-(trifluoro-methyl)pyridin-2-yl]urea (150 mg, 0.341 mmol) was slowly dissolved in THF (100 mL) by adding acetic acid (10-20 mL). The solution was further diluted with EtOH (300 mL) and run through the H-Cube® apparatus at 20 bar, rt, 1 mL/min. The resulting solution was concentrated then washed with satd. NaHCO3. A precititate formed and the desired product was collected by vacuum filtration to yield a tan solid. (150 mg, 99%). 1H-NMR (DMSO-d6) δ 11.89 (bs, 2H), 8.49 (d, J=5.0 Hz, 1H), 8.28 (s, 1H), 7.80 (s, 1H), 7.74 (d, J=8.8 Hz, 2H), 7.60 (s, 1H), 7.27 (m, 3H), 2.48 (q, J=7.8 Hz, 2H), 1.09 (t, J=7.5 Hz, 3H). MS [M+H]+=442.0; LCMS RT=2.95.

1. customrun through the H-Cube® apparatus at 20 bar, rt, 1 mL/min
2. concentrationThe resulting solution was concentrated
3. washthen washed with satd
4. customA precititate formed
5. filtrationthe desired product was collected by vacuum filtration
6. customto yield a tan solid
7. customLCMS RT=2.95