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Acetic Anhydride → HCID 13031642、化合物

HRID 1439381
ノート
印刷プレビュー

反応式

HRID 1439381 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:10](OC(=O)C)(=[O:12])[CH3:11]>N1C=CC=CC=1>[CH3:1][CH:2]1[C:7](=[O:8])[CH:6]=[CH:5][CH:4]([O:9][C:10](=[O:12])[CH3:11])[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

4

反応物 2

HCID 7918Acetic AnhydrideHCID 13011787HCID 13011787、化合物

生成物 1

HCID 13031642HCID 13031642、化合物収率 80%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A 12.8 g quantity of 2-methyl-6-hydroxy-3-oxo-3,6-dihydro-2H-pyran and 25 ml of acetic anhydride are reacted in the presence of 12.5 ml of pyridine with stirring at room temperature for 4 hours. After the reaction, the mixture is concentrated, the residue is poured into ice water, and the mixture is extracted with 100 ml 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 ethereal layer is concentrated, and the residue is distilled at a reduced pressure of 0.4 mm Hg to give 12.6 g of 2-methyl-6-acetoxy-3-oxo-3,6-dihydro-2H-pyran as a colorless liquid fraction at 80° to 83° C in a yield of 80%.

後処理

  1. customAfter the reaction
  2. concentrationthe mixture is concentrated
  3. additionthe residue is poured into ice water
  4. extractionthe mixture is extracted with 100 ml of ether
  5. washThe ethereal layer is washed with an aqueous solution of sodium carbonate
  6. dry with materialdried over magnesium sulfate
  7. customAfter removing the magnesium sulfate
  8. concentrationthe ethereal layer is concentrated
  9. distillationthe residue is distilled at a reduced pressure of 0.4 mm Hg

出典と根拠

ORDレコード
ord-25718068c7b944e3a0be902b5410be70
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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