Dichloromethane → HCID 22096864、化合物
反応式
S(Cl)([Cl:3])=O.O[CH2:6][CH2:7][N:8]([C:12]1[CH:22]=[CH:21][CH:20]=[CH:19][C:13]=1[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:9]CO.[CH2:23]([Cl:25])Cl>>[Cl:3][CH2:6][CH2:7][N:8]([C:12]1[CH:22]=[CH:21][CH:20]=[CH:19][C:13]=1[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:9][CH2:23][Cl:25]参加物
4
実験手順
Thionyl chloride (0.8 ml; 11.0 mmol) was added to a solution of 1.0 g (4.0 mmol) of ethyl 2-[N,N-bis(2-hydroxyethyl)amino]benzoate in 5 ml of methylene chloride, followed by stirring at room temperature for 1 hour. After the solvent was distilled out under reduced pressure, methylene chloride was added again in a small amount and was then distilled out under reduced pressure. This procedure was repeated twice. The resultant mixture was concentrated under reduced pressure, whereby 950 mg of a brown oil were obtained (yield: 83%).
後処理
- distillation