Sodium Carbonate → 4-Pyrimidinecarboxylic acid

HRID 273106

反応式

HRID 273106 の反応式
C[N:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH2:3]1.[Mn]([O-])(=O)(=O)=O.[K+].[C:14](=O)([O-:16])[O-:15].[Na+].[Na+]>O>[N:2]1[CH:7]=[CH:6][C:5]([C:14]([OH:16])=[O:15])=[N:4][CH:3]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 516875Potassium PermanganateHCID 18974088HCID 18974088、化合物

生成物 1

HCID 1693064-Pyrimidinecarboxylic acid収率 11%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3-Methyl-pyrimidine (9.41 g, 100 mmol), potassium permanganate (26.9 g) and sodium carbonate (10.6 g) was refluxed in water (100 ml) for 72 h followed by filtration through celite. The filtrate was washed with several portions of DCM and EtOAc before acidification with conc. HCl. The formed precipitate was collected and washed with water to yield 1.37 g of the title compound as a white solid. 1H NMR (DMSO-d6) d (ppm): 13.94 (br. s, 1H), 9.37 (d, 1H), 9.07 (d, 1H), 8.01 (dd, 1H).

後処理

  1. filtrationfollowed by filtration through celite
  2. washThe filtrate was washed with several portions of DCM and EtOAc before acidification with conc. HCl
  3. customThe formed precipitate was collected
  4. washwashed with water

出典と根拠

ORDレコード
ord-7cd744ccbfd14663aeb0ea21b33c2f20
出典データセット
uspto-grants-2008_11
特許番号
US07456200B2

関連ノート

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