Acetic Acid → HCID 85757965, compound

Participants

Reaction Steps

112.2 of acetic acid (96%) were added dropwise over 2 hours to a stirred mixture of 216.0 g (1 mol) of diisobutyl malonate, 250 g of 1,4-dioxane, 25.6 g of deionized water ad 80 g (1.15 mol) of sodium nitrite (technical grade), maintained at from 35° to 40° C. The mixture was allowed to continue reacting for 2 hours at 50° C., then 35.0 g of anhydrous sodium acetate and 200 g of methyl tert-butyl ether were added. After cooling of the mixture, the precipitated coarsely-crystalline sodium acetate trihydrate was filtered off and washed using methyl tert-butyl ether. Removal of the low-boilers by distillation at 60° C. under water-pump vacuum gave 258.7 g (88.6% of theory) of residue comprising primarily diisobutyl hydroxyiminomalonate. The content of unconverted diisobutyl malonate was 0.4 FID aea percent.

Provenance & Evidence