Trifluoromethyluracil → 5-Trifluoromethyl-2,4-bis(trimethylsilyloxy)pyrimidine

HRID 1734119ノート

反応式

HRID 1734119 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[C:4](=[O:10])[NH:5][C:6](=[O:9])[NH:7][CH:8]=1.[CH3:13][Si:14]([CH3:17])([CH3:16])Cl>C[Si](C)(C)N[Si](C)(C)C>[F:12][C:2]([F:11])([F:1])[C:3]1[C:4]([O:10][Si:14]([CH3:17])([CH3:16])[CH3:13])=[N:5][C:6]([O:9][Si:14]([CH3:17])([CH3:16])[CH3:13])=[N:7][CH:8]=1

参加物

4

反応物 2

HCID 5899TrifluoromethyluracilHCID 6397Chlorotrimethylsilane

生成物 1

HCID 109909625-Trifluoromethyl-2,4-bis(trimethylsilyloxy)pyrimidine

試薬・触媒・溶媒 1

HCID 13838Hexamethyldisilazane溶媒

実験手順

In 50 ml of hexamethyldisilazane, 6.16 g of 5-trifluoromethyluracil was suspended and then 0.22 ml of trimethylchlorosilane was added to the suspension, followed by heating the resulting mixture to reflux for 5 hours. After the reaction, the excess hexamethyldisilazane was removed by evaporation and the resultant was distilled in vacuum. All of the fractions of distillate obtained at about 60° C. under 1 mmHg were collected. Yield: 10.3 g

後処理

  1. temperatureby heating the resulting mixture
  2. temperatureto reflux for 5 hours
  3. customAfter the reaction
  4. customthe excess hexamethyldisilazane was removed by evaporation
  5. distillationthe resultant was distilled in vacuum
  6. customAll of the fractions of distillate obtained at about 60° C. under 1 mmHg
  7. customwere collected

出典と根拠

ORDレコード
ord-584c1ea662e0478e8b7213f4c54bf5ae
出典データセット
uspto-grants-1996_07
特許番号
US05532349

反応ノート

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