1,4-Dioxane → HCID 178516048, compound

Participants

Reaction Steps

First, 5.85 g of 4-[trans-4-(2,3-difluorophenyl)cyclohexyl]cyclohexanone ethylene ketal, 0.5 g of p-toluenesulfonic acid monohydrate, 35 ml of dioxane, and 105 ml of water were placed in a 200 ml flask. The mixture was stirred under reflux for 2 hours. The reaction mixture was extracted with ether. The ether layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=9/1), distilled under reduced pressure, and recrystallized from hexane to obtain 2.2 g of 4-[trans-4-(2,3-difluorophenyl)cyclohexyl]cyclohexanone (Y: 55.8%). The compound thus obtained had a purity of 98.1% by GC and a b.p. of 165° C./0.5 mmHg.

Provenance & Evidence