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HCID 13011787、化合物 → 6-Ethoxy-2-methyl-2H-pyran-3(6H)-one

HRID 1439378
ノート
印刷プレビュー

反応式

HRID 1439378 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 13011787HCID 13011787、化合物HCID 53630039Ethylorthoformate

生成物 1

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

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 241Benzene溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-c52ec922832d439da663bd0eb7aa25eb
出典データセット
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04059595

反応ノート

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