Potassium Carbonate → HCID 86696077, compound

Participants

Reaction Steps

Under a nitrogen atmosphere, a mixture of compound (91) (3.76 g, 10.80 mmol) and potassium carbonate (4.48 g, 32.4 mmol) was heated and agitated at 110° C. for 1 hour in a DMF (40 mL) solvent. Subsequently, 1-bromo-1-(bromodifluoromethyl)-4-propylcyclohexane (92) (7.21 g, 21.59 mmol) was added dropwise to the reaction mixture at 110° C., and the resultant mixture was further agitated for 3 hours. The reaction mixture was quenched with water, and extracted with 50 mL of toluene three times. Combined organic layers were washed with water and saturated brine, and then dried over magnesium sulfate, and a solvent was distilled off by an evaporator. The residue was purified by silica gel column chromatography, and thus 2-(difluoro(4-propylcyclohexa-1-en-1-yl)methoxy)-7-ethoxy-1,8,9,9,10,10-hexafluoro-9,10-dihydrophenanthrene (93) (4.40 g, yield 78.0%) was obtained.

Provenance & Evidence