Water → 2,3-Quinolinedicarboxylic acid

HRID 1462212

反応式

HRID 1462212 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 695082,3-Quinolinedicarboxylic acid

試薬・触媒・溶媒 1

HCID 10313272Nickel oxide (Ni2O3)触媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d57fc069928245d6b3ecaf62f5799d53
出典データセット
uspto-grants-1984_07
特許番号
US04459409

関連ノート

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