Nitric Acid → HCID 15132458, compound

Participants

Reaction Conditions

Reaction Steps

To a mixture of 8.94 g of 3-fluorodibenzothiophene S,S-dioxide in 100 ml of concentrated sulfuric acid, cooled at 18° C. in a water bath, was added dropwise 3.12 g of 71% nitric acid over 3 minutes. The mixture was stirred at room temperature for one hour, then poured over 500 ml of crushed ice and the solid collected, washed with water until neutral then dried at 100° C. This solid was dissolved in 200 ml of acetonitrile, treated with charcoal, filtered through diatomaceous earth and the filtrate concentrated to 110 ml producing successive crops of crystals. The first two crops were combined and recrystallized from 100 ml of acetonitrile, giving 7.56 g of the desired product as a solid, mp 275°-279° C.

Provenance & Evidence