反应详情

A solution of amine 84 (480 mg, 0.87 mmol) in DCM (8 mL) was treated with acetic anhydride (0.12 mL, 1.3 mmol) followed by DMAP (11 mg, 0.087 mmol). After 18 h, the solution was diluted with DCM, washed successively with 1M HCl, and brine, dried over anhydrous Na2SO4, filtered and concentrated to afford 86 (537 mg, 100%) as a white foam that was used without further purification. 1H NMR (CDCl3, 300 MHz): δ7.11-6.99 (m, 1H), 6.89 (br s, 1H), 6.74-6.67 (m, 1H), 6.61-6.56 (m, 1H), 4.77-4.69 (m, 1H), 4.63-4.57 (m, 2H), 4.39 (d, J=6.3 Hz, 1H), 4.10-3.95 (m, 2H), 3.82-3.67 (m, 2H), 3.54-3.48 (m, 1H), 3.45-3.36 (m, 1H), 2.87-2.79 (m, 4H), 2.44-2.38 (m, 1H), 2.23-2.08 (m, 6H), 1.65 (s, 1H), 1.49 (s, 9H), 1.32 (d, J=6.9 Hz, 3H), 0.99 (s, 9H) ppm.

1. washwashed successively with 1M HCl, and brine
2. dry with materialdried over anhydrous Na2SO4
3. filtrationfiltered
4. concentrationconcentrated