1-Bromo-6-fluoronaphthalene synthesis
- Product Name:1-Bromo-6-fluoronaphthalene
- CAS Number:59079-74-2
- Molecular formula:C10H6BrF
- Molecular Weight:225.06
116400-84-1
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Yield:59079-74-2 50%
Reaction Conditions:
with hydrogen tetrafluoroborate;NaNO2 in lithium hydroxide monohydrate at 80; for 1 h;
Steps:
83.6 Step 6:
C098-5 (1.5 g, 6.75 mmol) was dispersed in fluoroboric acid (15 mL), heated to 80 degrees to make the dispersion uniform, cooled to 0-5 degrees, and an aqueous solution of sodium nitrite (510 mg, 7.39 mmol) was added dropwise. , 0-5 degrees of stirring for 1h, TLC detection of raw materials basically complete the reaction. The reaction solution was filtered, washed with cold water, methanol and MTBE successively to a yellow solid, and dried to obtain 2.4 g of a yellow solid. Disperse 1.2 g of the above yellow solid in xylene (20 mL), and heat to reflux for 1 h. The reaction solution was cooled and concentrated, and the crude product was purified by silica gel column chromatography to obtain a colorless oil, which was solidified into a white solid C098-6 (380 mg, yield 50%).
References:
WO2022/17531,2022,A1 Location in patent:Page/Page column 106; 108
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