Triethoxysilane → HCID 86605938, compound

HRID 2378521Notes

Reaction equation

HRID 2378521 reaction equation
[F:1][C:2]([F:47])([F:46])[C:3]1[CH:45]=[CH:44][C:6]([CH2:7][C:8]2[CH:13]=[C:12]([O:14][CH2:15][CH2:16][CH:17]=[CH2:18])[CH:11]=[CH:10][C:9]=2[S:19]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH2:29][CH2:30][CH:31]=[CH2:32])=[CH:24][C:23]=2[CH2:33][C:34]2[CH:39]=[CH:38][C:37]([C:40]([F:43])([F:42])[F:41])=[CH:36][CH:35]=2)(=[O:21])=[O:20])=[CH:5][CH:4]=1.[CH2:48]([O:50][SiH:51]([O:55][CH2:56][CH3:57])[O:52][CH2:53][CH3:54])[CH3:49]>[Pt].C1(C)C=CC=CC=1>[F:47][C:2]([F:46])([F:1])[C:3]1[CH:45]=[CH:44][C:6]([CH2:7][C:8]2[CH:13]=[C:12]([O:14][CH2:15][CH2:16][CH2:17][CH2:18][Si:51]([O:55][CH2:56][CH3:57])([O:52][CH2:53][CH3:54])[O:50][CH2:48][CH3:49])[CH:11]=[CH:10][C:9]=2[S:19]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH2:29][CH2:30][CH2:31][CH2:32][Si:51]([O:55][CH2:56][CH3:57])([O:52][CH2:53][CH3:54])[O:50][CH2:48][CH3:49])=[CH:24][C:23]=2[CH2:33][C:34]2[CH:35]=[CH:36][C:37]([C:40]([F:42])([F:43])[F:41])=[CH:38][CH:39]=2)(=[O:20])=[O:21])=[CH:5][CH:4]=1

Participants

5

Reactant 2

HCID 13830TriethoxysilaneHCID 86605939HCID 86605939, compound

Product 1

HCID 86605938HCID 86605938, compound

Reagents, catalysts & solvents 2

HCID 23939PlatinumCatalystHCID 1140TolueneSolvent

Conditions

Temperature
100 °C

Procedure

After 0.61 g of 4-(trifluoromethyl)benzyl-4-(3-butenyloxy)phenyl sulfone and 20 mg of 10% platinum-active carbon were charged in a reaction vessel, and the inside of the vessel was then filled with nitrogen gas, 2 ml of triethoxysilane was added, and the mixture was then further stirred at 100° C. for 4 hours. After the reaction mixture was cooled to room temperature, 20 ml of toluene was added, and the mixture was filtered through a pad of Celite™. After the filtrate was concentrated, dehydrated ethanol was added to the residue, which was then left still over night. After precipitated crystal was removed by filtration, the filtrate was concentrated, and n-hexane was added to collect precipitated crystal by filtration. The obtained crystal was washed with n-hexane to produce 0.53 g of the desired product.

Workup

  1. additionwas added
  2. temperatureAfter the reaction mixture was cooled to room temperature
  3. filtrationthe mixture was filtered through a pad of Celite™
  4. concentrationAfter the filtrate was concentrated
  5. additionwas added to the residue, which
  6. waitwas then left still over night
  7. customAfter precipitated crystal
  8. customwas removed by filtration
  9. concentrationthe filtrate was concentrated
  10. additionn-hexane was added
  11. customto collect
  12. customprecipitated crystal
  13. filtrationby filtration
  14. washThe obtained crystal was washed with n-hexane

Sources & evidence

ORD record
ord-0b01069df78e4023ac52cba40a1dd1f1
Source dataset
uspto-grants-2008_12
Patent number
US07470803B2

Reaction notes

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