Dimethylformamide → HCID 22664951、化合物
反応式
P(Cl)(Cl)(Cl)=O.[CH2:6]([N:8]([C:10]1[CH:11]=[C:12]([OH:16])[CH:13]=[CH:14][CH:15]=1)[CH3:9])[CH3:7].CN([CH:20]=[O:21])C>>[CH2:6]([N:8]([C:10]1[CH:11]=[C:12]([OH:16])[C:13](=[CH:14][CH:15]=1)[CH:20]=[O:21])[CH3:9])[CH3:7]参加物
4
反応条件
- 温度
- 90 °C
実験手順
6.14 g (0.066 mol) of phosphorus oxychloride are cautiously added to 19 ml of dry DMF at −5° C. within a period of 5 minutes, during the course of which the temperature of the reaction solution should not exceed 10° C. Subsequently, a solution of 9.9 g (0.066 mol) of 3-(N-ethyl-N-methylamino)phenol in 14 ml of dry DMF is added thereto within a period of 10 minutes, during the course of which the temperature of the reaction solution should not exceed 20° C. When the addition is complete, the reaction solution is heated for 2 hours at 90° C. and then immediately poured onto 100 g of ice. The crude mixture is stirred for 30 minutes. The reaction solution is extracted three times with 100 ml of chloroform. The combined organic phases are concentrated under a high vacuum. The oily residue which remains is purified by column chromatography on silica gel (eluant n-hexanelchloroform 95:5). Yield: 5.8 g (26%), colourless solid.