Sulfate Ion → Bis(pentafluorophenyl)borinic acid

HRID 2415511ノート

反応式

HRID 2415511 の反応式
S([O-])([O-])(=O)=O.S([O-])([O-])(=O)=O.[Al+3].S([O-])([O-])(=O)=O.S([O-])([O-])(=O)=[O:18].[Al+3].[F:23][C:24]1[C:29]([B:30](C2C(F)=C(F)C(F)=C(F)C=2F)[C:31]2[C:36]([F:37])=[C:35]([F:38])[C:34]([F:39])=[C:33]([F:40])[C:32]=2[F:41])=[C:28]([F:53])[C:27]([F:54])=[C:26]([F:55])[C:25]=1[F:56]>C1(C)C=CC=CC=1>[F:23][C:24]1[C:29]([B:30]([C:31]2[C:36]([F:37])=[C:35]([F:38])[C:34]([F:39])=[C:33]([F:40])[C:32]=2[F:41])[OH:18])=[C:28]([F:53])[C:27]([F:54])=[C:26]([F:55])[C:25]=1[F:56]

参加物

5

反応物 3

HCID 1117Sulfate Ion2 回HCID 24850Aluminum SulfateHCID 582056Tris(pentafluorophenyl)borane

生成物 1

HCID 9841889Bis(pentafluorophenyl)borinic acid

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Moreover, that patent also discloses a method in which alminium sulfate 18 hydrate is used instead of water. Specifically, aluminium sulfate 18 hydrate is added to a toluene solution of tris (pentafluorophenyl) borane. After the solution is refluxed, insoluble alminium sulfate is separated from the reaction mixture. A solvent of a filtrate is removed in vacuo. Toluene is added to the thus obtained residue. After stirring, the insoluble matter passes through a G4 sintered-glass so as to be separated. The solvent of the filtrate is again removed in vacuo. Heptane is added to the residue. The solution is stirred and filtered so that a cake is obtained. Finally, the thus obtained cake is washed with heptane, and dried in vacuo so as to isolate bis (pentafluorophenyl) borinic acid. However, this method has such a problem that it is necessary to remove the by-product alminium sulfate and its process is so complicated.

後処理

  1. customis separated from the reaction mixture
  2. customA solvent of a filtrate is removed in vacuo
  3. additionToluene is added to the thus obtained residue
  4. customto be separated
  5. customThe solvent of the filtrate is again removed in vacuo
  6. additionHeptane is added to the residue
  7. stirringThe solution is stirred
  8. filtrationfiltered so that a cake
  9. customis obtained
  10. washFinally, the thus obtained cake is washed with heptane
  11. customdried in vacuo so as

出典と根拠

ORDレコード
ord-03415fdd158844aebd70c8ce41bb8f1a
出典データセット
uspto-grants-2004_11
特許番号
US06818785B2

反応ノート

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