反应详情

A mixture of compound 234c (885 mg, 1.99 mmol), ammonium formate (629 mg, 9.98 mmol), and Pd/C (89 mg, 10% w) in EtOH (16 mL) was refluxed for 1 hr. The reaction was then filtered though celite and concentrated under reduced pressure. The residue was diluted with DCM and washed with water. Organics were dried over Na2SO4, filtered, concentrated under reduced pressure, and purified by chromatography on silica gel (petroleum ether/EtOAc) to yield compound 236c as a white solid in 93% yield. 1H NMR (DMSO-d6, 400 MHz) δ (ppm) 2.54 (s, 3H), 3.94 (s, 3H), 7.06 (d, J=2.48 Hz, 1H), 7.37-7.40 (m, 2H), 8.02 (d, J=9.18 Hz, 1H), 8.97 (s, 1H), 11.89 (s, 1H).

1. temperaturewas refluxed for 1 hr
2. filtrationThe reaction was then filtered though celite and
3. concentrationconcentrated under reduced pressure
4. additionThe residue was diluted with DCM
5. washwashed with water
6. dry with materialOrganics were dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. custompurified by chromatography on silica gel (petroleum ether/EtOAc)