2-Methylpyridine → N-Methyl-N-(1-methylethyl)sulfamoyl chloride
反応式
[S:1](=[O:4])(=O)=[O:2].[N:5]1[CH:10]=CC=[CH:7][C:6]=1[CH3:11].CNC(C)C.P(Cl)(Cl)(Cl)(Cl)[Cl:18]>ClCCCl>[CH3:10][N:5]([CH:6]([CH3:11])[CH3:7])[S:1]([Cl:18])(=[O:4])=[O:2][S:1](=[O:4])(=O)=[O:2].[N:5]1[CH:10]=CC=[CH:7][C:6]=1[CH3:11].CNC(C)C.P(Cl)(Cl)(Cl)(Cl)[Cl:18]>ClCCCl>[CH3:10][N:5]([CH:6]([CH3:11])[CH3:7])[S:1]([Cl:18])(=[O:4])=[O:2]63.2 g (0.41 mol) of sulfur trioxide as a 52% solution in 1,2-dichloroethane were added with stirring at from 0 to 5° C. within 15 min to a solution of 70.0 g (0.752 mol) of α-picoline in 250 ml of 1,2-dichloroethane, followed by washing with 50 ml of 1,2-dichloroethane and stirring for 15 min until the temperature rose to 25° C. 26.3 g (0.342 mol) of 95% pure N-methyl-N-[1-methylethyl]amine were then added within 15 min with stirring at from 20 to 35° C., followed by washing with 50 ml of 1,2-dichloroethane and stirring at 55° C. for 15 min. After cooling to 20° C., 42.7 g (0.205 mol) of phosphorus pentachloride were added with stirring at from 20 to 32° C. within 15 min with external cooling, followed by washing with 150 ml of 1,2-dichloroethane. After stirring at 70° C. for 2 h, the reaction mixture was concentrated under reduced pressure and distilled via a Normag column head having a 10 cm column. 35 g (59.6% of theory) of the title compound having a boiling point of 110-115° C./30 mbar were obtained. Refractive index nD23=1.4620.
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