Dimethylamine → HCID 13726415、化合物
反応式
[CH3:1][NH:2][CH3:3].Cl[CH2:5][CH2:6][CH:7]1[CH2:13][N:12]([CH3:14])[C:11](=[S:15])[C:10]2[CH:16]=[C:17]([N+:20]([O-:22])=[O:21])[CH:18]=[CH:19][C:9]=2[O:8]1>>[CH3:1][N:2]([CH3:3])[CH2:5][CH2:6][CH:7]1[CH2:13][N:12]([CH3:14])[C:11](=[S:15])[C:10]2[CH:16]=[C:17]([N+:20]([O-:22])=[O:21])[CH:18]=[CH:19][C:9]=2[O:8]1参加物
3
実験手順
To 50 ml of freshly collected dimethylamine was added 4.25 g (0.014 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepine-5(4H)-thione. The reaction flask was sealed tightly and allowed to stand at room temperature for 6 days. The dimethylamine was evaporated at room temperature. The solid residue was taken up in methylene chloride, washed twice with 1N hydroxide and once with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. Approximately 0.8 g of the crude oil solid residue was triturated with isopropyl/ether to give the crystalline free base, m.p. 104°-109° C.
後処理
- customThe reaction flask was sealed tightly
- customThe dimethylamine was evaporated at room temperature
- washwashed twice with 1N hydroxide and once with water
- dry with materialdried over sodium sulfate