m-Chloroperbenzoic acid → HCID 21997628、化合物
反応式
[C:1]1([C:7]2[NH:12][C:11]3[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=3[S:9][C:8]=2[C:17]#[N:18])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.ClC1C=CC=C(C(OO)=[O:27])C=1>ClCCl>[C:1]1([C:7]2[NH:12][C:11]3[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=3[S:9](=[O:27])[C:8]=2[C:17]#[N:18])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1参加物
4
反応条件
- 温度
- 0 °C
実験手順
A mixture of 3-phenyl-4H-1,4-benzothiazine-2-carbonitrile (0.10 g) and 3-chloroperbenzoic acid (0.17 g, purity 80%) in dichloromethane (8 ml) was stirred at 0° C. for 30 min. The mixture was filtered and the filter cake was washed with dichloromethane and dried to give the title compound as pale crystals. Yield 66 mg; mp 182-184° C.; 1H-nmr(DMSO) δ (ppm): 12.31 (br, 1H), 8.09-7.99 (m, 1H), 7.83-7.60 (m, 7H), 7.60-7.48 (m, 1H); IR(KBr) ν (cm−1): 3211, 3161, 2985, 2935, 2850, 2193 (C≡N ), 1603, 1548, 1502, 1463, 1429, 1004, 771, 703; MS m/e (rel. intensity): 250 (86%; M+−16), 249 (87%), 218 (39%), 211 (100%), 190 (11%), 146 (23%), 108 (43%), 69 (43%).