Carbon Tetrachloride → HCID 75088899, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred solution of 60 g (0.92 mole) of nitrosyl chloride dissolved in 1300 ml of carbon tetrachloride at 5°-10° C. was added, over a period of 10 minutes, a solution of 60 g (0.4 mole) of p-methoxyacetophenone in 200 ml of carbon tetrachloride. The reaction mixture was then warmed to 35° C. and stirred at 35°-38° C. for 90 minutes during which the product precipitated (some cooling was necessary to maintain the temperature in the specified range). The reaction mixture was then warmed to 40° C. and after 15 minutes was cooled to 5° C. and filtered. The filter cake was washed with 400 ml of carbon tetrachloride and air-dried to provide 53.6 g (62.7% yield) of 1-chloro-1-p-methoxybenzoylformaldoxime as a white solid, m.p. 118°-125° C., which was sufficiently pure for further synthetic use.

Provenance & Evidence