Chloroacetyl chloride → HCID 178456413, compound

Participants

Reaction Conditions

Reaction Steps

19.8 g of malononitrile were dissolved in 30 ml of DMF and cooled to 0° C. While cooling, 87 g of tributylamine and 27 g of chloroacetyl 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 300 g of ice and 43 g of allylamine and stirred at room temperature for 8 hours. The precipitate was filtered off with suction, washed and dried. 38.1 g (78% of theory) of impure crude product were obtained and were boiled in 150 ml of isopropanol to purify. After cooling to 5° C., the precipitate was filtered off with suction, washed and dried. 31.2 g (64% of theory) of the compound of the formula ##STR26## of melting point 275° to 278° C. were obtained The IR, NMR, UV and mass spectra and the elemental analysis are consistent with the structural formula.

Provenance & Evidence