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7-Fluoronaphthalen-1-ol synthesis
- Product Name:7-Fluoronaphthalen-1-ol
- CAS Number:3132-92-1
- Molecular formula:C10H7FO
- Molecular Weight:162.16
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![Naphthalene, 1,4-dimethyl-2-phenyl-](/CAS/20210305/GIF/51036-91-0.gif)
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Yield:51036-91-0 300 g
Reaction Conditions:
with hydrogenchloride;methanol for 4 h;Inert atmosphere;Reflux;
Steps:
79.2 Step 2:
Under nitrogen protection,C094-1 (4.6g, 28.36mmol) was dissolved in methanol (90ml), concentrated hydrochloric acid (9ml) was added, heated to reflux for 4.0h, TLC showed that the reaction was complete (two new spots were generated, and the new spots were inseparable) . The reaction solution was concentrated, water was added, and saturated aqueous sodium bicarbonate solution was added dropwise to adjust the pH to neutrality, extracted with ethyl acetate, the organic phases were combined, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated, added with 30 ml of PE, stirred for 30 min, filtered, and the filtrate was Concentrated, the crude product was subjected to silica gel column chromatography to obtain a pale yellow solid mixture (1.5g, crude product) (by-products could not be separated from the preparation); the filter cake was washed and dried to obtain a white solid, which was dissolved by adding MIBE (3ml), and PE (20ml) was added dropwise under ultrasonication. , stirred at room temperature, a solid was precipitated, filtered, and the filter cake was washed and dried to obtain a white solid C094-2 (300 mg).
References:
WO2022/17531,2022,A1 Location in patent:Page/Page column 100-101
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![Naphthalene, 1,4-dimethyl-2-phenyl-](/CAS/20210305/GIF/51036-91-0.gif)
51036-91-0
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