3-ethynyl-2,4-difluoro-1,5-dimethoxybenzene synthesis
- Product Name:3-ethynyl-2,4-difluoro-1,5-dimethoxybenzene
- CAS Number:1453211-49-8
- Molecular formula:C10H8F2O2
- Molecular Weight:198.17
171290-52-1
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1453211-49-8
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1453211-50-1
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Yield:1453211-49-8 798 mg ，1453211-50-1 375 mg
Reaction Conditions:
with Selectfluor in acetonitrile at 20; for 12 h;Cooling with ice;
Steps:
4 Preparation Example 4
Preparation Example 4
A mixture of 1-ethynyl-3,5-dimethoxybenzene (4 g) and acetonitrile (80 mL) was ice cooled, and N-fluoro-N'-(chloromethyl)triethylenediamine bis(tetrafluoroborate) (19.4 g) was added thereto.
The resulting mixture was gradually warmed and stirred at room temperature for 12 hours.
To the reaction mixture, a saturated aqueous sodium hydrogen carbonate solution was added followed by extraction with ethyl acetate.
An organic layer obtained was washed with saturated brine, and then dried over anhydrous sodium sulfate and filtered.
After the filtrate was concentrated under reduced pressure, the resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane) and subsequently purified by silica gel column chromatography (chloroform/hexane) to give 3-ethynyl-2,4-difluoro-1,5-dimethoxybenzene (798 mg, Preparation Example No. PEx. 4-1, which is described later) and 1-ethynyl-2-fluoro-3,5-dimethoxybenzene (375 mg, Preparation Example No. PEx. 4-2, which is described later).
References:
US2014/142084,2014,A1 Location in patent:Paragraph 0263
![Benzene, 2,4-difluoro-1,5-dimethoxy-3-[2-(trimethylsilyl)ethynyl]-](/CAS/20210111/GIF/1560796-28-2.gif)
1560796-28-2
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1453211-49-8
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171290-52-1
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651734-54-2
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