反应详情

To a solution of CH2Cl2 (50 mL) was added of tert-butyl {4-[6-acetyl-4-amino-7-(morpholin-4-ylmethyl)pyrrolo[2,1-f][1,2,4]triazin-5-yl]-2 fluorophenyl}-carbamate (291 mg, 0.60 mmol) followed by trifluoroacetic acid (5 mL). The solution was allowed to stir for 30 min at rt. Aq saturated NaHCO3 was added to the solution until bubbling stopped. Additionally CH2Cl2 was added and the solution was then transferred to a separatory funnel. The organic layer was isolated while the aqueous layer was back extracted with CH2Cl2 (2×25 mL). The combined organic layers were collected, dried (MgSO4), filtered, and concentrated to dryness yielding 214 mg of the above compound as a white solid (0.56 mmol, yield 93%). 1H-NMR (DMSO-d6) δ 7.95 (s, 1H), 7.08 (dd, J=1.7 Hz, 10.3 Hz, 1H), 6.92 (dd, J=1.8 Hz, 7.9 Hz, 1H), 6.86 (t, J=8.7 Hz, 1H), 5.47 (s, 2H), 4.05 (s, 2H), 3.49 (m, 4H), 2.41 (m, 4H), 2.06 (s, 3H); MS [M+H]+=385.1; LCMS RT=1.16 min.

1. customuntil bubbling
2. additionAdditionally CH2Cl2 was added
3. customthe solution was then transferred to a separatory funnel
4. customThe organic layer was isolated while the aqueous layer
5. extractionwas back extracted with CH2Cl2 (2×25 mL)
6. customThe combined organic layers were collected
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated to dryness