反应详情

To a 20 mL vial which contained a solution of the product from step 1 (40 mg, 0.1 mmol) in dioxane (2 mL) was added HCl (4 N in dioxane, 2 mL) at 0° C. The mixture was allowed to warm to rt and stir at rt for 16 h. The solvent was removed and the crude was purified by recrystallization from MeOH-ether to yield the title product (30 mg, 90%); LCMS; 98%, ESI+ Calcd: 322.3, found m/z: 323.6 (M+1); 1HNMR (400 MHz, DMSO-d6): δ 1.73-1.84 (m, 1H), 1.86-2.04 (m, 2H), 2.10-2.20 (m, 1H), 3.18-3.28 (m, 2H), 3.88-3.98 (m, 1H), 4.16-4.21 (m, 1H), 4.33 (dd, J=10.8 Hz, 3.6 Hz, 1H), 7.14 (dd, J=6.8 Hz, 2.0 Hz, 2H), 7.40 (dd, J=6.8 Hz, 2.4 Hz, 2H), 7.89-7.97 (m, 4H).

1. customThe solvent was removed
2. customthe crude was purified by recrystallization from MeOH-ether