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Sodium Hydroxide → 5-Allyloxy-isophthalic acid monomethyl ester

HRID 2216750
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HRID 2216750 반응식
[CH2:1]([O:4][C:5]1[CH:6]=[C:7]([C:15]([O:17][CH3:18])=[O:16])[CH:8]=[C:9]([CH:14]=1)[C:10]([O:12]C)=[O:11])[CH:2]=[CH2:3].[OH-].[Na+]>CO>[CH2:1]([O:4][C:5]1[CH:14]=[C:9]([CH:8]=[C:7]([C:15]([O:17][CH3:18])=[O:16])[CH:6]=1)[C:10]([OH:12])=[O:11])[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 10933919Dimethyl 5-(allyloxy)isophthalate

생성물 1

HCID 219425375-Allyloxy-isophthalic acid monomethyl ester수율 74%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of dimethyl 5-allyloxy-isophthalate (3.7 g, 14.9 mmol) in methanol (75 mL) was treated with 1M sodium hydroxide (13.4 mL, 13.4 mmol) and the reaction stirred at room temperature for 16 hours. The mixture was concentrated under vacuum and the resulting residue was dissolved in water. The aqueous layer was washed with ethyl acetate (3×), and then acidified (pH 1) by the addition of aqueous HCl. The aqueous solution was then extracted with ethyl acetate. The organic extract was dried over anhydrous sodium sulfate, filtered and concentrated to afford 2.6 g (74%) of 3-allyloxy-5-(methoxycarbonyl)benzoic acid.

후처리

  1. concentrationThe mixture was concentrated under vacuum
  2. dissolutionthe resulting residue was dissolved in water
  3. washThe aqueous layer was washed with ethyl acetate (3×)
  4. additionby the addition of aqueous HCl
  5. extractionThe aqueous solution was then extracted with ethyl acetate
  6. extractionThe organic extract
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d0142b44e9c54bfe8a40a140bc7802f6
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07112595B2

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