Water → HCID 69425060, compound

Participants

Reaction Steps

Under exclusion of moisture, 3.8 g of 2-butyloxy-1,8-difluoro-6-propylfluoren-9-one (example 1) are dissolved in 50 ml of trifluoroacetic acid, and 4.6 ml of triethylsilane are added dropwise slowly at a temperature of 5-20° C. with gentle cooling. The mixture is subsequently stirred at room temperature for 1 h and then at 40-70° C. for 4 h. After cooling, the reaction mixture is added to water and extracted with dichloromethane. The combined org. phases are washed with water and 5% sodium hydrogencarbonate solution and dried over sodium sulfate. After the solvent has been removed in vacuo, the yellow residue is purified chromatographically on silica gel using 8:2 heptane/dichloromethane as eluent. After the solvent had been removed in vacuo, the product-containing fractions were recrystallized from heptane. 1.2 g of 2-butyloxy-1,8-difluoro-6-propylfluorene were obtained.

Provenance & Evidence