Chloride → HCID 23227573, compound

Participants

Reaction Steps

A 250 mL three-neck flask equipped with a magnetic stirrer, a thermometer and an addition funnel was charged with 50.8 g (400 mmoles) of oxalyl chloride and 75 mL of MTBE. Then to the resulting solution was slowly added 24.7 g (100 mmoles) of 95% di(3-hydroxy-1,1-dimethylbutyl) peroxide over a period of 30 minutes at 21°-30° C. The addition funnel was then replaced with a nitrogen gas tube and dry nitrogen gas wasslowly bubbled through the reaction mass in order to remove HCl over a period of 4 hours at 25°-30° C. The MTBE, excess oxalyl chloride, and any remaining gas were removed in vacuo using a water aspirator. Obtained was 38.2 g (97% of theory, uncorrected) of a amber liquid. An IR spectrum of the product showed no OH bands and showed a pairof carbonyl bands at 1790 cm-1 and 1755 cm-1. Based on hydrolyzable chloride content the assay of the product was 85.0% and the corrected yield was 82.7%.

Provenance & Evidence