2-Bromo-6-fluoronitrobenzene synthesis
- Product Name:2-Bromo-6-fluoronitrobenzene
- CAS Number:886762-70-5
- Molecular formula:C6H3BrFNO2
- Molecular Weight:220
7632-04-4
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Yield:-
Reaction Conditions:
in water;acetic acid at 55; for 4 h;
Steps:
11.1
To a suspension of sodium perborate tetrahydrate (135.374 g., 886.4 mmol) in 500 mL acetic acid at 55° C. was added dropwise a solution of 2-bromo-6-fluoro-phenylamine (33.685 g., 177.271 mmol) in 70 mL acetic acid over 1 hour. The reaction mixture was stirred at 55° C. for an additional 3 hours, then cooled to 0° C. in an ice bath. Insoluble materials were removed by filtration through a plug of celite, which was rinsed with 100 mL acetic acid. The combined acetic acid fractions were added to 3 L ice water with stirring to give a waxy solid which was removed by filtration. The crude solid was dissolved in 250 mL ethyl acetate, washed three times with 200 mL of 10% aqueous hydrogen chloride, 200 mL saturated sodium bicarbonate and 100 mL brine. The solution was concentrated in vacuo to give 11.51 g of 1-bromo-3-fluoro-2-nitro-benzene as a red oil, 1H NMR (CDCl3, 300 MHz) δ: 7.26 (m, 1H), 7.38 (m, 1H), 7.49 (m, 1H)
References:
Roche Palo Alto LLC US2007/15744, 2007, A1 Location in patent:Page/Page column 64-65
65896-11-9
295 suppliers
$6.00/1g
886762-70-5
221 suppliers
$11.00/1g