Methanol → Tetrahydropyran-4-ylacetic acid

HRID 129506

반응식

HRID 129506 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 2773575Tetrahydropyran-4-ylacetic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d62b7bd29474bb0903850b8dad8c0a0
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468740

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