反应详情

Trifluoroacetic acid (2.5 mL) was added to a solution tert-butyl (3R,7R)-1-(cyclopropylmethyl)-2-oxo-7-phenylazepan-3-ylcarbamate (82 mg, 0.23 mmol) in dichloromethane (5 mL). After 1 h, the mixture was concentrated and aqueous saturated sodium bicarbonate was added. The mixture was extracted with dichlormethane (2×), and the combined organic extracts were dried over magnesium sulfate, filtered, and concentrated to give the title compound (53 mg). 1H NMR (500 MHz, CDCl3) δ 7.40–7.37 (m, 2H), 7.34–7.31 (m, 3H), 4.97 (dd, J=9.3, 3.7 Hz, 1H), 4.05 (dd, J=9.8, 4.2 Hz, 1H), 3.24 (dd, J=14.4, 7.1 Hz, 1H), 2.69 (dd, J=14.2, 7.1 Hz, 1H), 2.16–2.10 (m, 2H), 2.03–1.97 (m, 1H), 1.92–1.85 (m, 2H), 1.65–1.56 (m, 1H), 0.69–0.63 (m, 1H), 0.34–0.23 (m, 2H), 0.09–0.04 (m, 1H), −0.10–0.15 (m, 1H).

1. concentrationthe mixture was concentrated
2. additionaqueous saturated sodium bicarbonate was added
3. extractionThe mixture was extracted with dichlormethane (2×)
4. dry with materialthe combined organic extracts were dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated