Water → 2,3-Quinolinedicarboxylic acid

HRID 1462212

반응식

HRID 1462212 반응식
[CH3:1][C:2]1[C:11]([C:12]([OH:14])=[O:13])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[OH2:15].[OH-:16].[Na+]>[O-2].[O-2].[O-2].[Ni+3].[Ni+3]>[N:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:10]=[C:11]([C:12]([OH:14])=[O:13])[C:2]=1[C:1]([OH:16])=[O:15]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 14819992-Methyl-3-quinolinecarboxylic acid

생성물 1

HCID 695082,3-Quinolinedicarboxylic acid

시약·촉매·용매 1

HCID 10313272Nickel oxide (Ni2O3)촉매

실험 절차

Three grams of 2-methylquinoline-3-carboxylic acid (0.012 mol of 3.5 hydrate) is dissolved in 100 ml 15% sodium hydroxide solution and an additional 100 ml H2O is added. The mixture becomes homogeneous. At room temperature is added, all at once, 12.0 g nickel peroxide, (0.044 mol, 3.6 eq, 20% excess) and the mixture is stirred magnetically for 12 hours. The insolubles are removed by vacuum filtration and washed with water. The filtrate is acidified to pH 2 and a solid fluffy precipitate forms. It is filtered and dried to give 2.48 g of quinoline-2,3-dicarboxylic acid which is hydrated with 1.3 moles H2O/mole compound as determined by NMR. Additional product is isolated from the aqueous filtrate by concentration and filtration. This brings the total actual product yield to 2.88 g of product having a melting point of 271°-277° C. Product yield is essentially quantitative.

후처리

  1. additionAt room temperature is added
  2. customThe insolubles are removed by vacuum filtration
  3. washwashed with water
  4. filtrationIt is filtered
  5. customdried

출처 및 근거

ORD 기록
ord-d57fc069928245d6b3ecaf62f5799d53
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04459409

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