反应详情

To a solution of (E)-3-[6-aminopyridin-3-yl]-N-methyl-N-(3-methyl-1H-inden-2-ylmethyl)acrylamide (0.159 g, 0.5 mmole), from Example 26, in anhydrous THF (20 mL) was added NaHCO3 (0.126 g, 1.5 mmole) followed by acetic anhydride (0.153 g, 0.15 mmole). The mixture was heated at reflux for 40 hr, then was concentrated under vacuum. The residue was partitioned between H2O and EtOAc, and the organic layer was dried over MgSO4, filtered and concentrated. The residue was triturated with diethyl ether to give the title compound (0.135 g, 74.8%) as an off-white solid: MS (ES) m/e 362.2 (M+H)+. Anal. Calcd for C22H23N3O2.0.25 H2O: C, 72.20; H, 6.47; N, 11.47. Found: C, 72.42; H, 6.45; N, 11.07.

1. temperatureThe mixture was heated
2. temperatureat reflux for 40 hr
3. concentrationwas concentrated under vacuum
4. customThe residue was partitioned between H2O and EtOAc
5. dry with materialthe organic layer was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was triturated with diethyl ether