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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 13011787, 화합물 → 6-Ethoxy-2-methyl-2H-pyran-3(6H)-one

HRID 1439378
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HRID 1439378 반응식
[CH3:1][CH:2]1[C:7](=[O:8])[CH:6]=[CH:5][CH:4]([OH:9])[O:3]1.C([O-])([O-])O[CH2:12][CH3:13]>C1C=CC=CC=1.[Cl-].[Zn+2].[Cl-]>[CH3:1][CH:2]1[C:7](=[O:8])[CH:6]=[CH:5][CH:4]([O:9][CH2:12][CH3:13])[O:3]1
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5

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HCID 13011787HCID 13011787, 화합물HCID 53630039Ethylorthoformate

생성물 1

HCID 145471086-Ethoxy-2-methyl-2H-pyran-3(6H)-one수율 85%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 241Benzene용매

실험 절차

A 12.8 g quantity of 2-methyl-6-hydroxy-3-oxo-3,6-dihydro-2H-pyran and 14.8 g of ethyl orthoformate are reacted in the presence of 1 g of zinc chloride in 100 ml of benzene with refluxing for 120 minutes. After the reaction, the benzene is distilled off, the residue is poured into 50 ml of water and the mixture is extracted three times with 50 ml portions of ether. The ethereal layer is washed with an aqueous solution of sodium carbonate and then dried over magnesium sulfate. After removing the magnesium sulfate, the dried mass is distilled to remove the ether, and the residue is distilled at a reduced pressure of 30 mm Hg to give 12 g of 2-methyl-6-ethoxy-3-oxo-3,6-dihydro-2H-pyran as a yellow liquid fraction at 82° to 85° C in a yield of 85%.

후처리

  1. temperaturewith refluxing for 120 minutes
  2. customAfter the reaction
  3. distillationthe benzene is distilled off
  4. additionthe residue is poured into 50 ml of water
  5. extractionthe mixture is extracted three times with 50 ml portions of ether
  6. washThe ethereal layer is washed with an aqueous solution of sodium carbonate
  7. dry with materialdried over magnesium sulfate
  8. customAfter removing the magnesium sulfate
  9. distillationthe dried mass is distilled
  10. customto remove the ether
  11. distillationthe residue is distilled at a reduced pressure of 30 mm Hg

출처 및 근거

ORD 기록
ord-c52ec922832d439da663bd0eb7aa25eb
출처 데이터셋
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04059595

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