5-BroMo-1,3-Difluoro-2-(PhenylMethoxy)-Benzene synthesis
- Product Name:5-BroMo-1,3-Difluoro-2-(PhenylMethoxy)-Benzene
- CAS Number:99045-18-8
- Molecular formula:C13H9BrF2O
- Molecular Weight:299.11
100-39-0
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104197-13-9
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$6.00/1g
99045-18-8
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$68.00/250mg
Yield:99045-18-8 95.8%
Reaction Conditions:
Stage #1: 4-bromo-2,6-difluorophenolwith potassium carbonate in N,N-dimethyl-formamide; for 0.166667 h;Inert atmosphere;
Stage #2: benzyl bromide in N,N-dimethyl-formamide at 20; for 4 h;Product distribution / selectivity;
Steps:
6.6.3.a
4-bromo-2,6-difluorophenol (5 g, 23.92 mmol) was dissolved in dimethylformamide (50 mL) in 250 ml round bottom flask equipped with argon atmosphere. Potassium carbonate (5 g, 35.55 mmol) was added and stirred for 10 minutes, followed by addition of benzyl bromide (4.5 g, 26.31 mmol) and stirred at ambient temperature for 4 h. TLC showed (hexane, Rf: 0.8) complete conversion of starting material. The reaction mixture was diluted with water (500 mL) and extracted with ethyl acetate (3 x 100 mL). The combined organic part was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford crude material, which was purified by column chromatography (silica gel: 100-200 mesh, eluent: 5% ethyl acetate in hexane) to afford the pure compound (7 g, 95.8%).
References:
WO2010/127856,2010,A1 Location in patent:Page/Page column 84
100-44-7
625 suppliers
$13.50/250G
104197-13-9
235 suppliers
$6.00/1g
99045-18-8
27 suppliers
$68.00/250mg
28177-48-2
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$15.00/5g
99045-18-8
27 suppliers
$68.00/250mg