Ammonia → HCID 178448398, 화합물

HRID 2057146노트

반응식

HRID 2057146 반응식
C(OP([O-])(OCC)=O)C.[C:10]([IH+:14]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:13])([CH3:12])[CH3:11].[F:25][C:26]1[C:31]([F:32])=[C:30]([F:33])[C:29]([F:34])=[C:28]([F:35])[C:27]=1[S:36]([OH:39])(=[O:38])=[O:37].N>C(Cl)Cl>[F:35][C:28]1[C:29]([F:34])=[C:30]([F:33])[C:31]([F:32])=[C:26]([F:25])[C:27]=1[S:36]([O-:39])(=[O:38])=[O:37].[C:21]([IH+:14]([C:10]([CH3:13])([CH3:12])[CH3:11])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:24])([CH3:23])[CH3:22]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 417247Barium pentafluorobenzenesulphonateHCID 178448396HCID 178448396, 화합물

생성물 1

HCID 178448398HCID 178448398, 화합물수율 76.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Di-tert-butylphenyliodonium diethylphosphate (546 mg; 1 mmol) and perfluorobenzenesulfonic acid (267 mg; 1.1 mmol) were dissolved in methylene chloride (10 ml), and 1% aqueous ammonia (10 ml) was added thereto. 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 435 mg of the target compound as white crystals (yield: 68%).

후처리

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

출처 및 근거

ORD 기록
ord-875d082fc7f947a996f4b91eefc938e5
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07335787B2

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