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

HRID 435197
ノート
印刷プレビュー

反応式

HRID 435197 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222Ammonia4 回HCID 962WaterHCID 11439SuccinimideHCID 13838Hexamethyldisilazane

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7c3bea7ec90b438ebe09a2a450737332
出典データセット
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04400509

反応ノート

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