Water → Bis(pentafluorophenyl)borinic acid

HRID 2414468

반응식

HRID 2414468 반응식
S([O-])([O-])(=O)=O.[Al+3].S([O-])([O-])(=O)=O.S([O-])([O-])(=O)=O.[Al+3].[OH2:18].[F:19][C:20]1[C:25]([B:26](C2C(F)=C(F)C(F)=C(F)C=2F)[C:27]2[C:32]([F:33])=[C:31]([F:34])[C:30]([F:35])=[C:29]([F:36])[C:28]=2[F:37])=[C:24]([F:49])[C:23]([F:50])=[C:22]([F:51])[C:21]=1[F:52]>C1(C)C=CC=CC=1>[F:19][C:20]1[C:25]([B:26]([C:27]2[C:32]([F:33])=[C:31]([F:34])[C:30]([F:35])=[C:29]([F:36])[C:28]=2[F:37])[OH:18])=[C:24]([F:49])[C:23]([F:50])=[C:22]([F:51])[C:21]=1[F:52]

참가 물질

5

반응물 3

HCID 962WaterHCID 24850Aluminum Sulfate2회HCID 582056Tris(pentafluorophenyl)borane2회

생성물 1

HCID 9841889Bis(pentafluorophenyl)borinic acid

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Moreover, that patent also discloses a method in which aluminum sulfate 18 hydrate is used instead of water. Specifically, aluminum sulfate 18 hydrate containing water of 1.77 molar equivalent vs. tris(pentafluorophenyl)borane is added to a toluene solution of tris(pentafluorophenyl)borane. After the solution is refluxed, insoluble aluminum sulfate is separated from the reaction mixture. A solvent of the filtrate is removed in vacuo. Toluene is added to the thus obtained residues. After stirring, the insoluble material is filtered 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 residues. 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 byproduct aluminum sulfate and its process is so complicated.

후처리

  1. temperatureAfter the solution is refluxed
  2. custominsoluble aluminum sulfate is separated from the reaction mixture
  3. customA solvent of the filtrate is removed in vacuo
  4. additionToluene is added to the thus obtained residues
  5. filtrationthe insoluble material is filtered through a G4 sintered-glass so as
  6. customto be separated
  7. customThe solvent of the filtrate is again removed in vacuo
  8. additionHeptane is added to the residues
  9. stirringThe solution is stirred
  10. filtrationfiltered so that a cake
  11. customis obtained
  12. washFinally, the thus obtained cake is washed with heptane
  13. customdried in vacuo so as

출처 및 근거

ORD 기록
ord-cf106301db9a4b18a2e158ee1f2c22c0
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06812360B2

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