تفاعل #2507821

معادلة التفاعل

potassium hydride

3-(4-bromo-2,5-difluorophenyl)-2-(6-fluoro-3-propylchroman-7-yl)propan-1-ol

ethanol

→

7-bromo-6,6′-difluoro-3′-propyl-3,4,3′,4′-tetrahydro-2H,2′H-[3,7′]-bichromenyl

المذيبات

ether

THF

THF

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed with sat. sodium chloride soln
2. 2
   تجفيفphase is dried over sodium sulfate
3. 3
   أخرىthe solvent is removed in vacuo
4. 4
   ترشيحthe crude product is filtered through silica gel with toluene
5. 5
   أخرىrecrystallised from heptane/ethyl acetate

الإجراء التجريبي

1.2 g (10.5 mmol) of potassium hydride (35 percent in paraffin oil) are initially introduced in 40 ml of THF, and a solution of 4.50 g (8.12 mmol) of 3-(4-bromo-2,5-difluorophenyl)-2-(6-fluoro-3-propylchroman-7-yl)propan-1-ol in 20 ml of THF is added dropwise at 30° C. The batch is subsequently stirred at 60° C. for 4 h, a little ethanol is added, and the batch is diluted with MTB ether and washed with sat. sodium chloride soln. The org. phase is dried over sodium sulfate, the solvent is removed in vacuo, and the crude product is filtered through silica gel with toluene and recrystallised from heptane/ethyl acetate, giving 7-bromo-6,6′-difluoro-3′-propyl-3,4,3′,4′-tetrahydro-2H,2′H-[3,7′]-bichromenyl as colourless crystals.

المصدر