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Saccharin → 2,5-Pyrrolidinedione, 1-(trimethylsilyl)-

HRID 435196
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HRID 435196 반응식
[CH3:1][Si:2]([CH3:9])([CH3:8])[NH:3][Si](C)(C)C.[C:10]1(=[O:16])N[C:13](=[O:15])[CH2:12][CH2:11]1.S1(C2C(=CC=CC=2)C(=O)N1)(=O)=O>C1(C)C=CC=CC=1>[CH3:1][Si:2]([CH3:9])([CH3:8])[N:3]1[C:13](=[O:15])[CH2:12][CH2:11][C:10]1=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5143SaccharinHCID 11439SuccinimideHCID 13838Hexamethyldisilazane

생성물 1

HCID 116654792,5-Pyrrolidinedione, 1-(trimethylsilyl)-수율 120,823.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

31.5 ml of hexamethyldisilazane (0.15 mmole) were added to a refluxing suspension of a mixture of 50 ml of toluene and 19.80 g (0.20 mole) of succinimide and 458 mg of saccharin (2.5 mmoles) and refluxing was continued for 2 hours. Fifteen minutes after the addition of the silylating agent, a clear, light yellow solution was obtained which turned brown when refluxing was continued. The reaction mixture was cooled, filtered and after evaporation of the solvent, the residue was vacuum distilled to obtain 31.04 g (90.8%) of N-trimethylsilylsuccinimide boiling at 86°-88° C. at 1.3 mm Hg.

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후처리

  1. temperaturerefluxing
  2. additionFifteen minutes after the addition of the silylating agent
  3. customa clear, light yellow solution was obtained which
  4. temperaturerefluxing
  5. temperatureThe reaction mixture was cooled
  6. filtrationfiltered
  7. customafter evaporation of the solvent
  8. distillationdistilled

출처 및 근거

ORD 기록
ord-e5956fc8cb834ccca62a044f337ce71b
출처 데이터셋
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04400509

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