二氯甲烷 → Bis(3,5-dimethylphenyl)-(4-fluorophenyl)-sulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate

HRID 1753690笔记

反应方程式

HRID 1753690 反应方程式
[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

参与物

5

反应物 3

HCID 6344二氯甲烷HCID 86664292Benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonateHCID 131733660Bis(3,5-dimethylphenyl)-(4-fluorophenyl)-sulfonium bromide

产物 1

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

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

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%.

后处理

  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

来源与证据

ORD记录
ord-1f1b24b1cf9045a29725523db8e2bbeb
来源数据集
uspto-grants-2015_10
专利号
US09164384B2

反应笔记

加载中…