Water → (Phenylsulfonylaminomethylene)bis(phosphonic acid)

HRID 1088605노트

반응식

HRID 1088605 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e200b1765a9b495f960f71e9133eddc3
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04963536

반응 노트

불러오는 중…