反应详情

16.5 g (59 mmol) of sodium metaborate octahydrate and 1.3 g (1.8 mmol) of bis(triphenylphosphine)palladium(II) chloride are initially introduced in 150 ml of water and 50 ml of THF, 12.5 g (38.5 mmol) of 3-(4′-bromo-3′-fluorobiphenyl-4-yl)propan-1-ol are added, and a solution of 12.5 g (0.053 mol) of 3-fluoro-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-phenol in 50 ml of THF is subsequently added dropwise. The batch is heated under reflux overnight, taken up in MTB ether and washed three times with water. The org. phase is dried over sodium sulfate, the solvent is removed in vacuo, and the crude product is recrystallised from toluene/ethyl acetate (9:1), giving 2,2′-difluoro-4″-(3-hydroxypropyl)[1,1′;4′,1″]-terphenyl-4-ol as colourless crystals.

1. temperatureThe batch is heated
2. temperatureunder reflux overnight
3. washwashed three times with water
4. dry with materialphase is dried over sodium sulfate
5. customthe solvent is removed in vacuo
6. customthe crude product is recrystallised from toluene/ethyl acetate (9:1)