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Methanol → Methyl 1-oxo-1,2-dihydroisoquinoline-3-carboxylate

HRID 1020011
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HRID 1020011 반응식
[C:1](O)(=O)[CH2:2][NH:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=O.[C:14](CC1C=CC=CC=1C=O)(O)=[O:15].[OH-:26].[K+].[CH3:28][OH:29]>>[O:26]=[C:4]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH:1]=[C:2]([C:28]([O:15][CH3:14])=[O:29])[NH:3]1
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참가 물질

4

반응물 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 866643832-Carboxymethylbenzaldehyde hippuric acid

생성물 1

HCID 641183Methyl 1-oxo-1,2-dihydroisoquinoline-3-carboxylate수율 99%

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온도
65 °C

실험 절차

The 2-carboxymethylbenzaldehyde hippuric acid adduct from above (1.0 g, 3.3 mmoles) was dissolved in methanol (20 mls) and solid potassium hydroxide (0.37 g, 6.6 mmoles) was added. The clear solution was heated (65° C.) for 1 hour. The reaction was evaporated and the solid residue partitioned between water (25 mls) and ethyl acetate (25 mls). The aqueous layer was further extracted with ethyl acetate (2×10 mls) and the combined ethyl acetate extracts washed with brine (10 mls) water (10 mls). After drying over magnesium sulphate the solution was evaporated to leave a yellow solid (0.68 g, 99% yield).

후처리

  1. customThe reaction was evaporated
  2. customthe solid residue partitioned between water (25 mls) and ethyl acetate (25 mls)
  3. extractionThe aqueous layer was further extracted with ethyl acetate (2×10 mls)
  4. washthe combined ethyl acetate extracts washed with brine (10 mls) water (10 mls)
  5. dry with materialAfter drying over magnesium sulphate the solution
  6. customwas evaporated

출처 및 근거

ORD 기록
ord-56c1c7c8a4854d16bb6e3ee30938b9b2
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716302B2

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