Sodium Carbonate → 4-Pyrimidinecarboxylic acid

HRID 273106

반응식

HRID 273106 반응식
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

참가 물질

5

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7cd744ccbfd14663aeb0ea21b33c2f20
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07456200B2

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