1,4-Dioxaspiro[4.4]nonane-7-carbonitrile synthesis
- Product Name:1,4-Dioxaspiro[4.4]nonane-7-carbonitrile
- CAS Number:159329-38-1
- Molecular formula:C8H11NO2
- Molecular Weight:153.18
41171-91-9
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159329-38-1
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Yield:159329-38-1 60%
Reaction Conditions:
with toluene-4-sulfonic acid;sodium sulfate in 1,2-dimethoxyethane; for 5 h;Reflux;
Steps:
1,4-dioxaspiro[4.4]nonane-7-carbonitrile (FOB04-42)
Dissolved FOB03-78 (1.00 g, 9.16 mmol) in 100 mL of toluene and subsequently added p-Toluenesulfonic acid (pTSA; 100 mg, 0.580 mmol) and ethylene glycol (2.56 mL, 45.82 mmol) to the reaction mixture followed by 10 g of Na2SO4 to remove water generated by the reaction. The reaction was stirred at reflux for 5 hrs and the Na2SO4 was then removed with a paper filter and an additional 10 g of Na2SO4 were added as well as an additional 5 eq. of ethylene glycol, the reaction was then allowed to stir at reflux overnight. The reaction solvent was then removed under reduced pressure and the crude purified via flash chromatography with solvent system ramping from 0% to 100% EtOAc in Hexanes, to yield 837 mg (60% yield) of the desired product as a colorless liquid.
References:
WO2020/210785,2020,A1 Location in patent:Paragraph 0168; 0172
930-30-3
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159329-38-1
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