Pyridine → HCID 54063699, 화합물

반응식

C[S:2]([CH2:5]CC#N)(=[O:4])=[O:3].P(Cl)(Cl)Cl.[N:13]1C=CC=[CH:15][CH:14]=1.[Cl:19]Cl.[CH2:21]([Cl:23])Cl>>[Cl:19][C:15](=[C:21]([Cl:23])[S:2]([CH3:5])(=[O:3])=[O:4])[C:14]#[N:13]

참가 물질

반응물 5

HCID 1049Pyridine2회

HCID 6344Dichloromethane

HCID 24387Phosphorus trichloride2회

HCID 24526Chlorine2회

HCID 12714644Dapansutrile

생성물 1

HCID 54063699HCID 54063699, 화합물수율 21%

실험 절차

31 g (0.23 mol) of 3-methylsulphonyl-propionitrile were melted at 100° C. in a 100 ml four-necked flask, and 2.2 g of PCl3 and 0.7 g of pyridine were added. 34 g of chlorine (0.48 mol) were then introduced at 100° C. during the course of 7 hours. After further addition of 1.1 g of PCl3 and 0.4 g of pyridine, 10 g of chlorine were again introduced. After cooling, the reaction mixture was diluted with 30 ml of methylene chloride and extracted twice by shaking with 50 ml of water in each case, and the organic phase was concentrated. 30 g of dark brown oil which, after mixing with a little ethanol, cooling and filtering off under suction, gave 9.5 g (21%) of pale crystals, melting point 110° to 114° C., without the yield of mother liquor.