1-Bromo-3-(difluoromethoxy)-5-fluorobenzene synthesis
- Product Name:1-Bromo-3-(difluoromethoxy)-5-fluorobenzene
- CAS Number:433939-28-7
- Molecular formula:C7H4BrF3O
- Molecular Weight:241.01
Yield:433939-28-7 79%
Reaction Conditions:
with potassium hydroxide in water;isopropyl alcohol at 20 - 85; for 18 h;
Steps:
25.iii (iii) 1-Bromo-3-fluoro-5-difluoromethoxybenzene
A mixture of 3-bromo-5-fluorophenol. (6.1 g, 31.0 mmol; see step (ii) above) and chlorodifluoromethane (13.0 g, 150.0 mmol) in i-PrOH (100 mL) and 30% KOH (80 mL) was heated in a sealed flask for 18 h at 80-85° C. The reaction mixture was cooled to room temperature and the layers were separated. The organic layer was concentrated in vacuo to afford a colourless oil. The aqueous layer was extracted with Et2O (3*30 mL). The crude oil and the combined organic extracts were washed with 2N NaOH (3*30 mL) and H2O (3*30 mL). The organics were then dried (Na2SO4), filtered through a small silica gel plug, and concentrated in vacuo to afford the sub-title compound (6.1 g, 79%) as a colourless oil that was used without further purification. 1H NMR (300 MHz, CDCl3) δ7.11-7.14 (m, 2H), 6.84 (dt, J=9 Hz, J=2 Hz, 1H), 6.50 (t, JH-F=72 Hz, 1H).
References:
US2004/19033,2004,A1 Location in patent:Page/Page column 32-33
433939-27-6
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1895-39-2
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433939-28-7
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433939-27-6
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65094-22-6
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433939-28-7
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$148.00/1g