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Water → 4-Hydroxyquinoline-3-carbaldehyde

HRID 2166880
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HRID 2166880 반응식
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[C:3]([C:12]#N)=[CH:2]1.[PH2]([O-])=[O:15].[Na+].O.N1C=CC=CC=1>C(O)(=O)C.[Ni]>[CH:12]([C:3]1[C:4](=[O:11])[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[NH:1][CH:2]=1)=[O:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 1049PyridineHCID 35393493-Quinolinecarbonitrile, 4-hydroxy-HCID 178527019HCID 178527019, 화합물

생성물 1

HCID 3481374-Hydroxyquinoline-3-carbaldehyde

시약·촉매·용매 2

HCID 935Nickel촉매
HCID 176
Acetic Acid
용매

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온도
60 °C

실험 절차

The 4-(1H)-quinolone-3-nitrile (12 g) and sodium hypophosphite (16.12 g) were dissolved in a mixture of acetic acid:water:pyridine=125 ml: 125 ml:250 ml and 4 g of Raney Nickel (W2 grade) added (Backeberg and Staskim, J.C.S. 1962, 3691). The reaction mixture was heated at 60° C. for four hours, then the hot suspension was filtered and the catalyst cake washed with warm ethanol into the filtrates. The combined filtrates and washings were evaporated to one-third of the original volume and on equal volume of water added. The precipitated solid was filtered off, washed with water and dried to give the required 3-formyl compound as a light-brown solid, m.p. 268°-270° C. (3-formyl-4(1H)-quinolone).

후처리

  1. filtrationthe hot suspension was filtered
  2. washthe catalyst cake washed with warm ethanol into the filtrates
  3. customThe combined filtrates and washings were evaporated to one-third of the original volume and on equal volume of water
  4. additionadded
  5. filtrationThe precipitated solid was filtered off
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-ed2bee7108794984b52290f90c41b884
출처 데이터셋
uspto-grants-1983_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04390541

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