Urea → HCID 178518523, 화합물

HRID 243865

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HRID 243865 반응식
[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]

참가 물질

5

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-705568b17178453dac59d6f41cc418a4
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653263B2

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