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Acetic Acid → HCID 66597026, 화합물

HRID 1811410
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HRID 1811410 반응식
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([CH:13]=O)=[C:9]2[C:4]=1[CH2:5][CH2:6][C:7](=[O:15])[NH:8]2.C(O)(=O)C>[C].[Pd].C(O)C>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([CH3:13])=[C:9]2[C:4]=1[CH2:5][CH2:6][C:7](=[O:15])[NH:8]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 86233763882023-34-9

생성물 1

HCID 66597026HCID 66597026, 화합물수율 89%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

실험 절차

5-Methoxy-2-oxo-1,2,3,4-tetrahydroquinoline-8-carboxaldehyde (1.00 g) and 10% palladium carbon (100 mg) were added to a mixed solvent of acetic acid (10 ml) and ethanol (10 ml), followed by catalytic reduction at 50° C. for 1 hour. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. The residue was subjected to extraction with ethyl acetate, and the extract was washed twice with water, washed with a saturated sodium chloride solution, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent to thereby obtain 826 mg (yield: 89%) of 5-methoxy-8-methyl-3,4-dihydro-1H-quinolin-2-one as a white powder.

후처리

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. extractionThe residue was subjected to extraction with ethyl acetate
  4. washthe extract was washed twice with water
  5. washwashed with a saturated sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent

출처 및 근거

ORD 기록
ord-adf90187e2814d62a03608af5cb0067a
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362252B2

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