反应详情

0.76 g of [4-(difluoromethoxy)-2,6-difluorophenyl]methanol (3.62 mmol, 1 eq.) were dissolved in 1.72 ml of 33% hydrogen bromide in glacial acetic acid (9.97 mmol, 2.75 eq.) and stirred at room temperature for 2 hours. 25 ml of diethyl ether were added and the mixture was stirred at room temperature for 15 min. The reaction mixture was added dropwise to 80 ml of aqueous saturated sodium hydrogen carbonate solution and stirred again at room temperature for 15 min. The separated aqueous layer was extracted twice with diethyl ether. The combined organic layers were washed with brine, dried over a silicone filter and concentrated in vacuo to yield 991 mg (3.56 mmol, 98.4%) of the analytically pure target compound.

1. stirringthe mixture was stirred at room temperature for 15 min
2. stirringstirred again at room temperature for 15 min
3. extractionThe separated aqueous layer was extracted twice with diethyl ether
4. washThe combined organic layers were washed with brine
5. dry with materialdried over a silicone
6. filtrationfilter
7. concentrationconcentrated in vacuo
8. customto yield 991 mg (3.56 mmol, 98.4%) of the analytically pure target compound