Hydrochloric Acid → 6-[2-(4-Piperidyl)ethyl]spiro[[1,3]dioxolo[4,5-f]isoindole-7,1'-cyclopropane]-5-one hydrochloride
反応式
[O:1]=[C:2]1[C:12]2[CH:11]=[C:10]3[O:13][CH2:14][O:15][C:9]3=[CH:8][C:7]=2[C:4]2([CH2:6][CH2:5]2)[N:3]1[CH2:16][CH2:17][CH:18]1[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]1.[ClH:31]>C(O)C>[ClH:31].[NH:21]1[CH2:22][CH2:23][CH:18]([CH2:17][CH2:16][N:3]2[C:4]3([CH2:6][CH2:5]3)[C:7]3[CH:8]=[C:9]4[O:15][CH2:14][O:13][C:10]4=[CH:11][C:12]=3[C:2]2=[O:1])[CH2:19][CH2:20]1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
To a reaction vessel, all compound XV obtained in the above step and 750 ml ethanol were added. The mixture was heated until dissolved completely, 36 ml concentrated hydrochloric acid was added, the reaction was kept at about 50-55° C. for 5 h, concentrated to about 200 ml under reduced pressure, 900 ml ethyl acetate was added dropwise, cooled and filtered, the filter cake was washed and dried, and 24.3 g compound II-5 was obtained, with yield of 46.2% (calculated according to compound IX-1). 1H NMR (D2O): δ 1.06 (t, 2H, J=6.7 Hz), 1.32-1.46 (m, 6H), 1.60 (m, 1H), 1.91 (d, 2H, J=13.5 Hz), 2.91-3.03 (m, 4H), 3.39 (d, 2H, J=12.8 Hz), 5.90 (s, 2H), 6.18 (s, 1H), 6.68 (s, 1H); MS (ESI): m/z 315 [M-Cl]+.