Chloroacetyl chloride → HCID 20064396, compound

Participants

Reaction Conditions

Reaction Steps

99 g of malononitrile were dissolved in 150 ml of DMF and cooled to 0° C. While cooling, 306 g of triethylamine and 159 g of chloracetyl chloride were simultaneously added dropwise to this, and the mixture was stirred at 10° C. for 10 minutes. The mixture was then added to a mixture of 1.5 kg of ice and 291 g of 2-methoxyethylamine and stirred at room temperature for 8 hours. The volatiles were removed by distillation at 100° C. under atmospheric pressure, and the distillation residue was concentrated in a rotary evaporator at the water pump. The residue was recrystallized from 500 ml of isopropanol. The precipitate was filtered off with suction, washed and dried at 50° C. 205.5 g (76% of theory) of the compound of the formula ##STR27## of melting point 108° to 110° C. were obtained. The IR, NMR, UV and mass spectra and the elemental analysis are consistent with the structural formula.

Provenance & Evidence