Dichloromethane → HCID 14324551, compound

Participants

Reaction Conditions

Reaction Steps

To one liter of dichloromethane was added 800 g of 4-chloro-3-nitrobenzenesulfonyl chloride prepared in the above step and the mixture was cooled to 0° C. Then, a mixture of 600 g of hexadecylamine, 251 ml of triethylamine, and 780 ml of dichloroethane was added dropwise to the mixture at 20° C. to 30° C. After performing the reaction for 2 hours at room temperature, the dichloromethane was distilled off from the reaction mixture under reduced pressure and the residue was dissolved in 3 liters of methanol under heating. After gradually cooling the solution to room temperature to form crystals, 3 liters of methanol was added to the solution and the mixture was ice-cooled to deposit crystals which were then recovered by filtration and dried to provide 1020 g of the above-described compound with a yield of 88%. The melting point thereof was 91° C. to 93° C.

Provenance & Evidence