反应详情

To a stirred solution of the compound obtained from step I (0.45 g, 1.12 mmol) in dichloromethane (1.1 mL) at 0° C. was added trifluoroacetic acid (1.1 mL). The reaction mixture was gradually warmed to room temperature and stirred for 1 h. The volatiles were removed under vacuum and the residue was triturated several times with diethyl ether to obtain 2-[(3-aminotricyclo[3.3.1.03,7]non-1-yl)methyl]-1H-isoindole-1,3(2H)-dione (0.4 g) as its trifluoroacetic acid salt in 86% yield. m/z (M+1) 297; 1H NMR (DMSO-d6) 300 MHz δ 8.05 (s (br), 2H), 7.92-7.80 (m, 4H), 3.51 (s, 2H), 2.38-2.30 (m, 1H), 2.30-2.22 (m, 1H), 1.85-1.66 (m, 6H), 1.60-1.50 (m, 3H), 1.45-1.38 (m, 1H).

1. customThe volatiles were removed under vacuum
2. customthe residue was triturated several times with diethyl ether