Water → 1,6-Dihydro-2-(2-fluoroanilino)-6-oxo-5-pyrimidinecarboxylic acid

HRID 979135

反応式

HRID 979135 の反応式
[F:1][C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][C:3]=1[NH:4][C:5]1[NH:6][C:7](=[O:16])[C:8]([C:11]([O:13]CC)=[O:12])=[CH:9][N:10]=1.[OH-].[Na+].O>C(O)(=O)C>[F:1][C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][C:3]=1[NH:4][C:5]1[NH:6][C:7](=[O:16])[C:8]([C:11]([OH:13])=[O:12])=[CH:9][N:10]=1

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 13562811Ethyl 1,6-dihydro-2-(2-fluoroanilino)-6-oxo-5-pyrimidinecarboxylate

生成物 1

HCID 139135241,6-Dihydro-2-(2-fluoroanilino)-6-oxo-5-pyrimidinecarboxylic acid収率 69%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Ethyl 1,6-dihydro-2-(2-fluoroanilino)-6-oxo-5-pyrimidinecarboxylate (5 g) and sodium hydroxide (2 g) are added to water (100 ml), and the mixture is refluxed with stirring for 1 hour. After cooling, the reaction mixture is acidified with acetic aicd, and the resulting solid is collected by filtration and recrystallized from DMF. The precipitate is collected by filtration and added to water (70 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-fluoroanilino)-6-oxo-5-pyrimidinecarboxylic acid (3.1 g). M.p. 300° 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. filtrationThe precipitate is collected by filtration
  6. additionadded to water (70 ml)
  7. temperaturethe mixture is refluxed
  8. stirringwith stirring for 1 hour
  9. temperatureAfter cooling
  10. filtrationthe resulting product is collected by filtration
  11. customdried at 80° C. under reduced pressure

出典と根拠

ORDレコード
ord-41de55184250445fa8daccd79170a3a0
出典データセット
uspto-grants-1987_05
特許番号
US04666915

関連ノート

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