反应详情

温度

90 °C

Sodium hydroxide (0.2′1 mL of 1 N, 0.2 mmol) was added to a solution of methyl (5R,6S)-rel-13-cyclohexyl-6,7-dihydro-5,6-dihydroxy-5H-indolo[2,1-a][2]benzazepine-10-carboxylate (20 mg, 0.049 mmol) in methanol (0.5 mL) and tetrahydrofuran (0.5 mL) in a microwave vial. The vial was sealed and the contents heated at 90° C. for 7 min in a microwave apparatus. The solution was acidified with dilute hydrochloric acid and a precipitate was observed to form. The solid was collected by filtration and purified on the Prep. reverse phase HPLC. The product containing fraction was concentrated on a Speed Vac® to leave the titled compound as a white solid (18 mg, 94%). ESI-MS m/z 392 (MH+) 1H NMR (500 MHz, MeOD) δ 1.25-1.34 (m, 1 H) 1.39-1.54 (m, 2 H) 1.60-1.67 (m, 1 H) 1.77-1.86 (m, 2H) 1.93-2.00 (m, 1 H) 2.01-2.17 (m, 3 H) 2.93-3.02 (m, 1 H) 3.36 (m, 1 H) 4.43 (d, J=4.27 Hz, 1 H) 4.54 (m, 1 H) 4.72 (dd, J=14.19, 7.17 Hz, 1 H) 7.46 (m, 2 H) 7.53 (m, 1 H) 7.74 (dd, J=8.39, 1.37 Hz, 1 H) 7.79 (d, J=7.63 Hz, 1 H) 7.90 (d, J=8.24 Hz, 1 H) 8.19 (s, 1 H).

1. customThe vial was sealed
2. customto form
3. filtrationThe solid was collected by filtration
4. custompurified on the Prep
5. additionThe product containing fraction
6. concentrationwas concentrated on a Speed Vac®