Ammonia → Triphenylsulfonium 4-trifluoromethylbenzenesulfonate

HRID 1168018노트

반응식

HRID 1168018 반응식
[Br-].[C:2]1([S+:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])([O-])OCC.[F:27][C:28]([F:40])([F:39])[C:29]1[CH:34]=[CH:33][C:32]([S:35]([OH:38])(=[O:37])=[O:36])=[CH:31][CH:30]=1.N>C(Cl)Cl>[F:40][C:28]([F:27])([F:39])[C:29]1[CH:30]=[CH:31][C:32]([S:35]([O-:38])(=[O:36])=[O:37])=[CH:33][CH:34]=1.[C:15]1([S+:8]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 98779144-(Trifluoromethyl)benzene-1-sulfonic acidHCID 11984010Triphenylsulfonium BromideHCID 53630039Ethylorthoformate

생성물 1

HCID 22057398Triphenylsulfonium 4-trifluoromethylbenzenesulfonate수율 76.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triphenylsulfonium bromide (343 mg; 1 mmol), ethyl orthoformate (296 mg; 2 mmol), and 4-trifluoromethylbenzenesulfonic acid (271 mg; 1.2 mmol) were dissolved in methylene chloride (10 ml), and the mixture was stirred for 6 hours at room temperature. The reaction mixture was alkalinized by adding 1% aqueous ammonia (10 ml), and subjected to extraction with methylene chloride three times, followed by drying. The solvent was removed through distillation, to thereby yield solid matter. The solid matter was washed and stirred in ether, to thereby yield 375 mg of the target compound as white crystals (yield: 76%).

후처리

  1. extractionsubjected to extraction with methylene chloride three times
  2. customby drying
  3. customThe solvent was removed through distillation
  4. customto thereby yield solid matter
  5. washThe solid matter was washed
  6. stirringstirred in ether

출처 및 근거

ORD 기록
ord-4deead9a253c4c639072d07990e31915
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620957B1

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