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Acetic Acid → 5-Pyrimidinecarboxylic acid, 1,4-dihydro-2-((2-ethoxyphenyl)amino)-4-oxo-

HRID 979123
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HRID 979123 반응식
[CH2:1]([O:3][C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[NH:6][C:7]1[NH:8][C:9](=[O:18])[C:10]([C:13]([O:15]CC)=[O:14])=[CH:11][N:12]=1)[CH3:2].[OH-].[Na+].C(O)(=O)C>O>[CH2:1]([O:3][C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[NH:6][C:7]1[NH:8][C:9](=[O:18])[C:10]([C:13]([OH:15])=[O:14])=[CH:11][N:12]=1)[CH3:2]
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참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 13562776Ethyl 1,6-dihydro-2-(2-ethoxyanilino)-6-oxo-5-pyrimidinecarboxylate

생성물 1

HCID 30627055-Pyrimidinecarboxylic acid, 1,4-dihydro-2-((2-ethoxyphenyl)amino)-4-oxo-수율 64.8%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Ethyl 1,6-dihydro-2-(2-ethoxyanilino)-6-oxo-5-pyrimidinecarboxylate (3.4 g) and sodium hydroxide (1 g) are added to water (50 ml), and the mixture is refluxed with stirring for 1 hour. After cooling, the reaction mixture is acidified with acetic acid, and the resulting solid is collected by filtration and recrystallized from DMF. The precipitate thus obtained is added to water (50 ml), and the mixture is refluxed with stirring for 1 hour. After cooling, the resulting product is collected by filtration and dried at 80° C. under reduced pressure to give 1,6-dihydro-2-(2-ethoxyanilino)-6-oxo-5-pyrimidinecarboxylic acid (2 g). M.p. 226°-228° C.

후처리

  1. temperaturethe mixture is refluxed
  2. temperatureAfter cooling
  3. filtrationthe resulting solid is collected by filtration
  4. customrecrystallized from DMF
  5. customThe precipitate thus obtained
  6. temperaturethe mixture is refluxed
  7. stirringwith stirring for 1 hour
  8. temperatureAfter cooling
  9. filtrationthe resulting product is collected by filtration
  10. customdried at 80° C. under reduced pressure

출처 및 근거

ORD 기록
ord-1b19a7d30bda4e11b605edaabfb2ee02
출처 데이터셋
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04666915

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