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Water → 2-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid

HRID 61814
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HRID 61814 반응식
C([O:3][C:4](=[O:20])[C:5]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH:15]([CH3:17])[CH3:16])=[C:10]([O:18][CH3:19])[CH:9]=1)([CH3:7])[CH3:6])C.[OH-].[Na+].O>C1COCC1.CCO>[CH:15]([O:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]([CH3:7])([CH3:6])[C:4]([OH:20])=[O:3])=[CH:9][C:10]=1[O:18][CH3:19])([CH3:16])[CH3:17]
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참가 물질

6

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 66834644HCID 66834644, 화합물

생성물 1

HCID 668346712-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

2-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid ethyl ester (Compound L3-1, 1.45 g, 5.17 mmol) was dissolved in THF (13 mL) and EtOH (13 mL), added with 1 N aqueous solution of sodium hydroxide (10.3 mL, 2.0 eq.), and stirred at 80° C. overnight. The reaction solution was added to water and extracted with ethyl acetate. The aqueous layer was acidified by using 1 N aqueous solution of hydrochloric acid, extracted with ethyl acetate, washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the target compound (white solid, 1.10 g, 84%).

후처리

  1. extractionextracted with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. customThe drying agent was removed by filtration
  6. customthe residues obtained
  7. concentrationafter concentration under reduced pressure
  8. customwere purified by silica gel column chromatography (ethyl acetate/hexane)
  9. customto obtain the target compound (white solid, 1.10 g, 84%)

출처 및 근거

ORD 기록
ord-f865c7d0fe7f44da81d69c156db8f76c
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09440922B2

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