Urea → HCID 178518523、化合物

HRID 1193120ノート

反応式

HRID 1193120 の反応式
[NH2:1][C:2]([NH2:4])=[O:3].C([O:7][C:8](=O)[CH:9]([F:15])[C:10](OCC)=[O:11])C.CC[O-].[Na+]>CCO>[F:15][C:9]1[C:8]([OH:7])=[N:1][C:2]([OH:3])=[N:4][C:10]=1[OH:11]

参加物

5

反応物 3

HCID 1176UreaHCID 12702Diethyl fluoromalonateHCID 2723922Sodium ethoxide

生成物 1

HCID 178518523HCID 178518523、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a heterogeneous mixture of urea (641 mg, 10.67 mmol) and diethylfluoromalonate (1.96 g, 10.67 mmol) in EtOH (11 mL) was added 2.68 M NaOEt in EtOH (7.96 mL, 21.34 mmol). The mixture was heated at reflux for 60 h and then allowed to cool to room temperature. The mixture was filtered and the cake was then dissolved in warm water and the resulting solution was acidified with concentrated HCl to pH 2. The mixture was allowed to cool to room temperature and then cooled in an ice bath before filtering. The cake was washed with water and dried to afford 5-fluoropyrimidine-2,4,6-triol as a slightly off white solid (1.45 g, 93%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 60 h
  3. filtrationThe mixture was filtered
  4. dissolutionthe cake was then dissolved in warm water
  5. temperatureto cool to room temperature
  6. temperaturecooled in an ice bath
  7. filtrationbefore filtering
  8. washThe cake was washed with water
  9. customdried

出典と根拠

ORDレコード
ord-6be81dfbb4c04744ba8766d243fb6e9c
出典データセット
uspto-grants-2014_03
特許番号
US08680275B2

反応ノート

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