Methanol → Tetrahydropyran-4-ylacetic acid

HRID 129506

反応式

HRID 129506 の反応式
CO.[OH-].[Na+].[O:5]1[CH2:10][CH2:9][CH:8]([CH2:11][C:12]([O:14]CC)=[O:13])[CH2:7][CH2:6]1>O>[O:5]1[CH2:10][CH2:9][CH:8]([CH2:11][C:12]([OH:14])=[O:13])[CH2:7][CH2:6]1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 2773412Ethyl tetrahydropyran-4-ylacetate

生成物 1

HCID 2773575Tetrahydropyran-4-ylacetic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

20 ml of methanol, 10 ml of water and 1 g of sodium hydroxide were added to 0.9 g of ethyl 4-tetrahydropyranylacetate and agitated at 80° C. for 1 hour. The solvent was removed by distillation, to which water was added. After washing with ethyl acetate, a hydrochloric acid aqueous solution was added to the resultant aqueous phase to an extent of pH of 3, followed by extraction with chloroform under salting-out conditions and drying with anhydrous magnesium sulfate. This was removed by filtration and the solvent was distilled off, thereby obtaining 0.87 g of a crude intended compound.

後処理

  1. customThe solvent was removed by distillation, to which water
  2. additionwas added
  3. washAfter washing with ethyl acetate
  4. additiona hydrochloric acid aqueous solution was added to the resultant aqueous phase to an extent of pH of 3
  5. extractionfollowed by extraction with chloroform under salting-out conditions
  6. dry with materialdrying with anhydrous magnesium sulfate
  7. customThis was removed by filtration
  8. distillationthe solvent was distilled off
  9. customobtaining 0.87 g of a crude intended compound

出典と根拠

ORDレコード
ord-7d62b7bd29474bb0903850b8dad8c0a0
出典データセット
uspto-grants-1995_11
特許番号
US05468740

関連ノート

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