Dichloromethane → 1-Methoxy-1,3,3-trimethylurea
反応式
Cl.[CH3:2][N:3](C)[OH:4].Cl[CH2:7]Cl.[CH3:9][N:10]([CH3:14])[C:11](Cl)=[O:12]>CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[CH3:7][O:4][N:3]([CH3:2])[C:11]([N:10]([CH3:14])[CH3:9])=[O:12]Cl.[CH3:2][N:3](C)[OH:4].Cl[CH2:7]Cl.[CH3:9][N:10]([CH3:14])[C:11](Cl)=[O:12]>CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[CH3:7][O:4][N:3]([CH3:2])[C:11]([N:10]([CH3:14])[CH3:9])=[O:12]A mixture of dimethylhydroxylamine hydrochloride (150.0 g, 1.54 mol), 4-dimethylaminopyridine (9.4 g, 0.076 mol), and dichloromethane (1.35 L) was chilled to −20° C., under argon. Dimethylcarbamyl chloride (135 ml, 1.46 mol) and pyridine (315 ml) were added consecutively over 25 minutes. The reaction was slowly warmed to room temperature over 2 hours, and agitated for about 16 hours. The reaction mixture was filtered to remove pyridine hydrochloride, and concentrated by rotary evaporator. The mixture was diluted with t-butyl methyl ether (500 ml), and the solids were removed by filtration. The filtrate was concentrated by rotary evaporation. Vacuum distillation provided the desired product (135.10 g, 69%) as a colorless oil.
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