Dichloromethane → Bis(3,5-dimethylphenyl)-(4-fluorophenyl)-sulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate

HRID 1753690노트

반응식

HRID 1753690 반응식
[F:1][C:2]([F:13])([S:9]([O-:12])(=[O:11])=[O:10])[CH:3]([OH:8])[C:4]([F:7])([F:6])[F:5].C([N+](C)(C)C)C1C=CC=CC=1.[Br-].[CH3:26][C:27]1[CH:28]=[C:29]([S+:34]([C:42]2[CH:47]=[C:46]([CH3:48])[CH:45]=[C:44]([CH3:49])[CH:43]=2)[C:35]2[CH:40]=[CH:39][C:38]([F:41])=[CH:37][CH:36]=2)[CH:30]=[C:31]([CH3:33])[CH:32]=1.C(Cl)Cl>O>[F:13][C:2]([F:1])([S:9]([O-:12])(=[O:10])=[O:11])[CH:3]([OH:8])[C:4]([F:5])([F:7])[F:6].[CH3:48][C:46]1[CH:47]=[C:42]([S+:34]([C:29]2[CH:30]=[C:31]([CH3:33])[CH:32]=[C:27]([CH3:26])[CH:28]=2)[C:35]2[CH:36]=[CH:37][C:38]([F:41])=[CH:39][CH:40]=2)[CH:43]=[C:44]([CH3:49])[CH:45]=1

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 86664292Benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonateHCID 131733660Bis(3,5-dimethylphenyl)-(4-fluorophenyl)-sulfonium bromide

생성물 1

HCID 131733662Bis(3,5-dimethylphenyl)-(4-fluorophenyl)-sulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate수율 92%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 21 g of benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate synthesized according to the method of JP-A 2012-107151, the solution containing bis(3,5-dimethylphenyl)-(4-fluorophenyl)-sulfonium bromide obtained in Synthesis Example 1-47, 30 g of methylene chloride, and 50 g of deionized water was stirred for 30 minutes. The organic layer was separated, washed with water, and concentrated in vacuum. To the residue, diisopropyl ether was added for recrystallization. The resulting crystals were collected by filtration and dried in vacuum, obtaining 26 g of the target compound, bis(3,5-dimethylphenyl)-(4-fluorophenyl)sulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate as white crystals. Yield 92%.

후처리

  1. customsynthesized
  2. customThe organic layer was separated
  3. washwashed with water
  4. concentrationconcentrated in vacuum
  5. additionTo the residue, diisopropyl ether was added for recrystallization
  6. filtrationThe resulting crystals were collected by filtration
  7. customdried in vacuum

출처 및 근거

ORD 기록
ord-1f1b24b1cf9045a29725523db8e2bbeb
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09164384B2

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