反应详情

To a solution of the intermediate from step A (1.13 g, 3.7 mmol) in DMF (20 mL) was added hydrazine (0.37 mL, 4.07 mmol, 35% aqueous solution). After 2 hours the reaction mixture was concentrated in vacuo. The residue was suspended in H2O (20 mL). A white precipitate crashed out. The aqueous layer was extracted with ethyl acetate (2×). The organic layer was dried over anhydrous Na2SO4, filtered and concentrated in vacuo. An off-white solid was obtained. This material was used in the next step without any further purification. 1H NMR (CDCl3, 500 MHz): δ 7.7 (d, J=1.8 Hz, 2H), 7.66 (d, J=8.4 Hz, 2H), 7.35 (s, 1H), 7.03 (d, J=8.7 Hz, 2H), 6.8 (s, 1H), 3.91 (s, 3H). LC-MS: 2.92 min. (M+H)=319.

1. concentrationAfter 2 hours the reaction mixture was concentrated in vacuo
2. extractionThe aqueous layer was extracted with ethyl acetate (2×)
3. dry with materialThe organic layer was dried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customAn off-white solid was obtained
7. customThis material was used in the next step without any further purification
8. custom2.92 min. (M+H)=319