Sulfuric Acid → HCID 20563131, compound

Participants

Reaction Steps

A 500 ml. reactor equipped with mechanical stirrer, nitrogen inlet, condenser, thermometer and addition funnel is charged with 102.0 grams (1.2 equivalents) of cyanoacetic acid and 225.0 grams (2.2 equivalents) of concentrated sulfuric acid. Stirring is begun and nitrogen is blanketed over the stirred solution. The reactor is then placed in a water bath to provide temperature control. Upon dissolution of the cyanoacetic acid, the solution temperature is adjusted to 25° C. and 101.0 grams (0.6 equivalents) of a 60 percent by weight active aqueous solution of N-methylol acrylamide is added dropwise through the addition funnel while agitation continues. The rate of addition and water bath temperature are adjusted so that the reacting materials are maintained at 30° C.±2° C. The addition takes approximately 1.5 hours. After completion of the N-methylol acrylamide addition, the reacting materials are maintained at 30° C.±2° C. with agitation for an additional 1.5 hours for the completion of the reaction.

Provenance & Evidence