Hexamethyldisilazane → HCID 22223251、化合物

HRID 1744763

反応式

HRID 1744763 の反応式
[CH3:1][C:2]1[C:3](=[O:10])[NH:4][C:5](=[O:9])[NH:6][C:7]=1[CH3:8].[CH3:11][Si](C)(C)N[Si](C)(C)C>CN(C=O)C>[CH3:11][N:6]1[C:7]([CH3:8])=[C:2]([CH3:1])[C:3](=[O:10])[NH:4][C:5]1=[O:9]

参加物

4

反応物 2

HCID 13838HexamethyldisilazaneHCID 960315,6-Dimethyluracil

生成物 1

HCID 22223251HCID 22223251、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

6.00 g (42.9 mmol) 5,6-dimethyluracil was dissolved in 26 mL of hexamethyldisilazane and 2.1 mL DMF. The mixture was heated for 11 hours at 150° C. and the excess of hexamethyldisilazane was removed under reduced pressure. Toluene was added to the mixture and evaporated off under reduced pressure to remove any residual hexamethyldisilazane. The residue was dissolved in 25 mL of iodomethane, refluxed for 2 hours, the excess iodomethane then evaporated off under reduced pressure and the residue recrystallized from deionised water yielding after drying 5.76 g (87%) of 1,5,6-trimethyluracil (m.p. 254–257° C., lit. 256–258° C.).

後処理

  1. customthe excess of hexamethyldisilazane was removed under reduced pressure
  2. additionToluene was added to the mixture
  3. customevaporated off under reduced pressure
  4. customto remove any residual hexamethyldisilazane
  5. dissolutionThe residue was dissolved in 25 mL of iodomethane
  6. temperaturerefluxed for 2 hours
  7. customthe excess iodomethane then evaporated off under reduced pressure
  8. customthe residue recrystallized from deionised water yielding
  9. dry with materialafter drying 5.76 g (87%) of 1,5,6-trimethyluracil (m.p. 254–257° C., lit. 256–258° C.)

出典と根拠

ORDレコード
ord-aaa8c976615b4462a9470aef40471c31
出典データセット
uspto-grants-2006_03
特許番号
US07018786B2

関連ノート

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