Ammonia → Triphenylsulfonium toluenesulfonate

HRID 2057144노트

반응식

HRID 2057144 반응식
COP([O-])(OC)=O.[C:8]1([I+][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)C=CC=CC=1.[C:21]1(C)[CH:26]=[CH:25][C:24]([S:27]([OH:30])(=[O:29])=[O:28])=[CH:23][CH:22]=1.N>C(Cl)Cl>[C:23]1([CH3:8])[C:24]([S:27]([O-:30])(=[O:28])=[O:29])=[CH:25][CH:26]=[CH:21][CH:22]=1.[C:15]1([S+:27]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:24]2[CH:23]=[CH:22][CH:21]=[CH:26][CH:25]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 6101p-Toluenesulfonic acidHCID 22995015Diphenyliodonium dimethylphosphate

생성물 1

HCID 22257397Triphenylsulfonium toluenesulfonate수율 98.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Diphenyliodonium dimethylphosphate (315 mg; 1 mmol) and p-toluenesulfonic acid (189 mg; 1.1 mmol) were dissolved in methylene chloride (10 ml), and the mixture was stirred, followed by addition of 1% aqueous ammonia (10 ml). After the alkalinity of the solution was confirmed, the solution was stirred vigorously. The thus-obtained mixture was allowed to stand, and the aqueous layer was separated. The aqueous layer was washed with water successively until the aqueous layer exhibited neutral pH. The methylene chloride solution was dried, and the solvent was removed through distillation. The residue was washed in ether by stirring, to thereby precipitate 214 mg of the target compound as white crystals (yield: 84%).

후처리

  1. stirringthe solution was stirred vigorously
  2. customthe aqueous layer was separated
  3. washThe aqueous layer was washed with water successively until the aqueous layer
  4. dry with materialThe methylene chloride solution was dried
  5. customthe solvent was removed through distillation
  6. washThe residue was washed in ether
  7. stirringby stirring

출처 및 근거

ORD 기록
ord-55fcff100a0443d393bc4b084acae5cb
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07335787B2

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