Water → (Phenylsulfonylaminomethylene)bis(phosphonic acid)

HRID 1088605ノート

反応式

HRID 1088605 の反応式
[C:1]1([S:7]([NH:10][CH:11]([P:20](=[O:27])([O:24]CC)[O:21]CC)[P:12](=[O:19])([O:16]CC)[O:13]CC)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.I[Si](C)(C)C.O.C(Cl)(Cl)Cl>C(Cl)Cl>[C:1]1([S:7]([NH:10][CH:11]([P:20](=[O:21])([OH:27])[OH:24])[P:12](=[O:13])([OH:19])[OH:16])(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 6212ChloroformHCID 85247Trimethylsilyl iodideHCID 53933859Tetraethyl(phenylsulfonylaminomethylene)bis(phosphonate)

生成物 1

HCID 10068042(Phenylsulfonylaminomethylene)bis(phosphonic acid)収率 64.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tetraethyl (phenylsulfonylaminomethylene)bis(phosphonate) (400 mg) in methylene chloride (4 ml), was added iodotrimethylsilane (0.8 ml) dropwise with stirring under nitrogen gas atmosphere in an ice-water bath. The mixture was stirred for 30 minutes at the same condition and then at ambient temperature for 1.5 hours. To the reaction mixture were added water (10 ml) and chloroform (8 ml) under ice-water bath cooling. The separated aqueous layer was washed with chloroform until its color disappeared and then evaporated in reduced pressure. The residue was washed with ethanol to give white powder of (phenylsulfonylaminomethylene)bis(phosphonic acid) (194 mg).

後処理

  1. stirringThe mixture was stirred for 30 minutes at the same condition
  2. temperaturecooling
  3. washThe separated aqueous layer was washed with chloroform until its color
  4. customevaporated in reduced pressure
  5. washThe residue was washed with ethanol

出典と根拠

ORDレコード
ord-e200b1765a9b495f960f71e9133eddc3
出典データセット
uspto-grants-1990_10
特許番号
US04963536

反応ノート

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