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Ethyl bromoacetate → (1,3-benzodioxol-5-yloxy)acetic acid

HRID 1700247
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HRID 1700247 반응식
[CH2:1]1[O:5][C:4]2[CH:6]=[C:7]([OH:10])[CH:8]=[CH:9][C:3]=2[O:2]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:18][C:19]([O:21]CC)=[O:20]>CC(C)=O>[CH2:1]1[O:2][C:3]2[CH:9]=[CH:8][C:7]([O:10][CH2:18][C:19]([OH:21])=[O:20])=[CH:6][C:4]=2[O:5]1
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참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 68289Sesamol

생성물 1

HCID 1531512(1,3-benzodioxol-5-yloxy)acetic acid수율 11.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

The mixture of sesamol (270 mg, 2.0 mmol), potassium carbonate (910 mg, 6.6 mmol), ethyl bromoacetate (2.55 ml, 22.9 mmol) and acetone (25 ml) was refluxed for 21 h. After cooling, the mixture was filtered to remove potassium carbonate. The filtrate was concentrated under reduced pressure. To this residue, 20 ml dioxane and 14 ml 5% sodium hydroxide solution were added. After the uiixture was stirred at room temperature overnight, it was acidified with concentrated hydrochloric acid to pH 2, and then extracted three times with ethyl acetate (20 ml each). Organic phases were combined, washed with water and brine, dried over magnesium sulfate, filtered, and then evaporated in vacuo. The residue was recrystallized from chloroform and acetone to give 45 mg 3,4-methylenedioxyphenoxyacetic acid as white crystals, mp 149-151 ° C.

후처리

  1. temperaturewas refluxed for 21 h
  2. temperatureAfter cooling
  3. filtrationthe mixture was filtered
  4. customto remove potassium carbonate
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. additionTo this residue, 20 ml dioxane and 14 ml 5% sodium hydroxide solution were added
  7. extractionextracted three times with ethyl acetate (20 ml each)
  8. washwashed with water and brine
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. customevaporated in vacuo
  12. customThe residue was recrystallized from chloroform and acetone

출처 및 근거

ORD 기록
ord-eece8e3ec94043cf9e52ed4b152a5068
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350756B1

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