반응 #357836

반응 방정식

2-thiopheneethanol

1,3-dioxolane

→

title compound

수율 60.3%

6,7-dihydro-4H-thieno[3,2-c]pyrane

수율 60.3%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도the resulting mixture was refluxed for 10 hours
2. 2
   농축concentrated by evaporation under reduced pressure
3. 3
   workup.ADDITIONTo the residue, 100 mL of water and 150 mL of n-hexane were added
4. 4
   기타The organic layer was separated
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   농축concentrated under reduced pressure
7. 7
   workup.DISTILLATIONThe residue was distilled under reduced pressure

실험 절차

10.0 g of 2-thiopheneethanol, 11.5 g of 1,3-dioxolane, and 862 mg of indium(III) chloride were added to 780 mL of acetonitrile, and the resulting mixture was refluxed for 10 hours. The reaction product solution was cooled to room temperature and concentrated by evaporation under reduced pressure. To the residue, 100 mL of water and 150 mL of n-hexane were added, and the resulting mixture was stirred for 5 minutes. The organic layer was separated and dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was distilled under reduced pressure to obtain 6.6 g (yield of 60%) of the title compound, of which analysis data were the same as obtained in Example 14.

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