1,2-Dichloroethane → HCID 22310829, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 12.5 g (12.5 moles) of the N-oxide of 3 methoxy-4-nitropyridine, 7.72 ml (1.1 eq.) of methyl sulfate and 70 ml of 1,2-dichloroethane is heated at 70° C. for 2.5 hours. It is allowed to cool and 70 ml of water are added. It is cooled in a salt and ice bath and, in portions, 7.55 g (2.1 moles) of sodium cyanide are added, controlling the temperature so as not to exceed 10° C. After 4 hours stirring, the reaction mixture is extracted with ethyl ether, the organic phase is washed with water, concentrated and the residue chromatographed (ethyl acetate/dichloromethane). There is obtained 7.06 g of a yellow oil (yield 53%).

Provenance & Evidence