Water → Triphenylsulfonium 2-pivaloyloxy-1,1-difluoroethanesulfonate

HRID 908077

반응식

HRID 908077 반응식
O.[C:2]([O:8][CH2:9][C:10]([F:16])([F:15])[S:11]([O-:14])(=[O:13])=[O:12])(=[O:7])[C:3]([CH3:6])([CH3:5])[CH3:4].[Na+].[I-].[C:19]1([S+:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>ClCCl>[C:2]([O:8][CH2:9][C:10]([F:16])([F:15])[S:11]([O-:14])(=[O:12])=[O:13])(=[O:7])[C:3]([CH3:6])([CH3:5])[CH3:4].[C:32]1([S+:25]([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 21881071Triphenylsulfonium iodideHCID 57817346Sodium 2-pivaloyloxy-1,1-difluoroethanesulfonate

생성물 1

HCID 86632753Triphenylsulfonium 2-pivaloyloxy-1,1-difluoroethanesulfonate수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 700 g of dichloromethane and 400 g of water were dissolved 159 g (0.37 mole) of sodium 2-(pivaloyloxy)-1,1-difluoroethanesulfonate (purity 63%) and 132 g (0.34 mole) of triphenylsulfonium iodide. The organic layer was separated, washed three times with 200 g of water, and concentrated. Diethyl ether was added to the residue for recrystallization, obtaining the target compound as white crystals. 164 g (yield 95%).

후처리

  1. customThe organic layer was separated
  2. washwashed three times with 200 g of water
  3. concentrationconcentrated
  4. additionDiethyl ether was added to the residue for recrystallization

출처 및 근거

ORD 기록
ord-65c768594a3b4c2cb513e02524d0e1f1
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017302B2

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