Methyl iodide → HCID 86740645、化合物
反応式
[CH3:1][O:2][P:3]([O:13]C)([N:5]=[C:6]([S:10][CH2:11][CH3:12])[N:7]([CH3:9])[CH3:8])=[S:4].[CH3:15]I>CO>[CH3:1][O:2][P:3]([S:13][CH3:15])([N:5]=[C:6]([S:10][CH2:11][CH3:12])[N:7]([CH3:9])[CH3:8])=[O:4]参加物
4
実験手順
A mixture of 36.8 g of N'-(dimethoxyphosphinothioyl)-N,N-dimethylcarbamimidothioic acid, ethyl ester, 120 ml of methanol and 5.0 g of methyl iodide was heated under reflux for 18 hours, then another 5.0 g of methyl iodide was added and heating under reflux was continued for 6 hours. The mixture was concentrated under vacuum, the residue dissolved in methylene chloride, the methylene chloride solution washed once with water and dried over anhydrous magnesium sulfate. The solvent was removed in a rotary evaporator and the residual oil distilled in a Kugelrohr (bath temperature 140° C., pressure 0.3 mm) yielding 23.8 g (65% of theoretical) of N'-(methoxy(methylthio)phosphinyl)-N,N-dimethylcarbamimidothioic acid, ethyl ester. The IR and NMR spectra are in agreement with the assigned structure and identical to those obtained from the compound prepared by the method A.