Dimethylamine → HCID 59355185、化合物
反応式
CS(O[CH2:6][CH2:7][N:8]1[CH2:12][C:11]([CH3:14])([CH3:13])[NH:10][C:9]1=[O:15])(=O)=O.[CH3:16][NH:17][CH3:18]>O1CCCC1>[CH3:16][N:17]([CH3:18])[CH2:6][CH2:7][N:8]1[CH2:12][C:11]([CH3:14])([CH3:13])[NH:10][C:9]1=[O:15]参加物
4
実験手順
In a sealed tube, a solution of 2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)ethyl methanesulfonate (500 mg, 2.1 mmol) and dimethyl amine (4.6 mmol) in tetrahydrofuran (2.3 mL) was heated at 60° C. for 5 hours. Additional dimethylamine (1 mL of a 2M tetrahydrofuran solution) was added and the reaction was heated for 3 additional hours. The solution was concentrated to a crude residue under reduced pressure, then dissolved in 5 mL of 1 N HCl. The aqueous solution was washed with dichloromethane, then made basic (pH>8) with sodium carbonate and extracted with dichloromethane twice. The aqueous solution was further adjusted to pH>10 with NaOH, and extracted with twice with dichloromethane. The combined organic fractions were dried over sodium sulfate and concentrated under reduced pressure to give 316 mg of an off-white solid. 1H NMR (CDCl3, 400 MHz) δ 1.30 (s, 6H), 2.27 (s, 6H), 2.41-2.45 (t, 6.8 Hz, 2H) 3.24 (s, 2H), 3.29-3.33 (t, J=6.8 Hz, 2H), 3.51-3.61 (m, 14H), 3.88 (br m, 2H), 7.27-7.29 (d, J=8.1 Hz, 2H), 7.58-7.60 (d, J=8.2 Hz, 2H); LRMS (ESI/APCI) m/z 186 [M+H]+.