Hexamethyldisilazane → HCID 22223251, 화합물

HRID 1744763

반응식

HRID 1744763 반응식
[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]

참가 물질

4

반응물 2

HCID 13838HexamethyldisilazaneHCID 960315,6-Dimethyluracil

생성물 1

HCID 22223251HCID 22223251, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

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.).

후처리

  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.)

출처 및 근거

ORD 기록
ord-aaa8c976615b4462a9470aef40471c31
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07018786B2

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