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

HRID 979123
ノート
印刷プレビュー

反応式

HRID 979123 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1b19a7d30bda4e11b605edaabfb2ee02
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04666915

反応ノート

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