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

HRID 435197
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HRID 435197 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.N.O>ClCCl>[CH3:1][Si:2]([CH3:9])([CH3:8])[N:3]1[C:13](=[O:15])[CH2:12][CH2:11][C:10]1=[O:16]
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참가 물질

6

반응물 4

HCID 222Ammonia4회HCID 962WaterHCID 11439SuccinimideHCID 13838Hexamethyldisilazane

생성물 1

HCID 116654792,5-Pyrrolidinedione, 1-(trimethylsilyl)-수율 119.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

15.6 ml (0.075 mole) of hexamethyldisilazane were added dropwise over a few minutes to a refluxing suspension of 9.90 g (0.1 mole) of succinimide and 0.24 g (0.5 mmole) of di-4-nitrophenyl N-4-toluenesulfonyl-phosphoramidate in 50 ml of dichloromethane and a stream of nitrogen was led over the reaction mixture to pass the ammonia evolved into water. The progress of the reaction was established by titration of the ammonia evolved and it was found that after refluxing for 1.5 hours, the production of ammonia was completed. 90% of the theoretical amount of ammonia had been evolved and refluxing was continued for another 2 hours. Then the solvent was removed by distillation at normal pressure and fractionation under reduced pressure yielded 15.36 g (89.8%) of N-trimethylsilylsuccinimide boiling at 118°-119° C. at 18 mm Hg and nD 25=1.4745.

후처리

  1. temperaturethat after refluxing for 1.5 hours
  2. temperaturerefluxing
  3. customThen the solvent was removed by distillation at normal pressure and fractionation under reduced pressure

출처 및 근거

ORD 기록
ord-7c3bea7ec90b438ebe09a2a450737332
출처 데이터셋
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04400509

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