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

HRID 1753690ノート

反応式

HRID 1753690 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-1f1b24b1cf9045a29725523db8e2bbeb
出典データセット
uspto-grants-2015_10
特許番号
US09164384B2

反応ノート

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