m-Chloroperbenzoic acid → HCID 53880775、化合物
反応式
[CH3:1][N:2]([CH2:4][C:5]#[C:6][C:7]1[C:13]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=2[S:11][C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]=2[CH:8]=1)[CH3:3].ClC1C=CC=C(C(OO)=[O:31])C=1>C(Cl)(Cl)Cl>[CH3:1][N+:2]([O-:31])([CH2:4][C:5]#[C:6][C:7]1[C:13]2[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=2[S:11][C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]=2[CH:8]=1)[CH3:3]参加物
4
実験手順
A solution of 2 g. of N,N-dimethyl-3-(8-chloro-dibenzo [b,f]thiepin-10-yl)-2-propynylamine in 100 ml. chloroform is treated at -50° C. with 1.2 g. of m-chloroperbenzoic acid. The solution is stirred for 15 minutes at this temperature, warmed to room temperature and chromatographed on basic aluminum oxide using chloroform/methanol (9:1) as the eluant, whereby there is obtained N,N-dimethyl-3-(8-chloro-dibenzo [b,f]thiepin-10-yl)-2-propynylamine N-oxide, which melts at 68°-69° C. after recrystallization from ethyl acetate/petroleum ether.