Dichloromethane → 4-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonate

HRID 1672115Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1672115
[F:1][C:2]([F:17])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:12])([F:11])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].O[C:19]1[CH:24]=[CH:23][C:22]([S+:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:21][CH:20]=1.ClCCl.C(N(CC)[C:44](Cl)=[O:45])C.[CH2:49]([N:51](CC)[CH2:52][CH3:53])[CH3:50]>O>[F:17][C:2]([F:1])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:11])([F:12])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].[CH2:49]([N:51]([O:14][C:44]([C:19]1[CH:24]=[CH:23][C:22]([S+:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:21][CH:20]=1)=[O:45])[CH2:52][CH3:53])[CH3:50]

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 6916Diethylcarbamoyl chlorideHCID 8471TriethylamineHCID 22481373HCID 22481373, Verbindung

Produkt 1

HCID 866361064-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonateAusbeute 152 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Into a flask, 30 g of 4-hydroxyphenyldiphenylsulfonium perfluorobutanesulfonate and 300 g of dichloromethane were added to prepare a solution. In the flask, a nitrogen gas was blown. To the solution, 17.9 g of N,N-diethylcarbamoyl chloride was added and then 10.5 g of triethylamine was added thereto. The resultant mixture was stirred at room temperature for 1 hour. To the obtained reaction mixture, 100 g of ion-exchanged water was added and an organic layer was obtained by separation. The obtained organic layer was washed with 300 mL of distillated water and then dried over anhydrous magnesium sulfate. Magnesium sulfate was removed by filtration and the obtained filtrate was concentrated. The obtained residue was dried under reduced pressure to obtain 26.7 g of 4-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonate.

Aufarbeitung

  1. customto prepare a solution
  2. additionwas added
  3. customan organic layer was obtained by separation
  4. washThe obtained organic layer was washed with 300 mL of distillated water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customMagnesium sulfate was removed by filtration
  7. concentrationthe obtained filtrate was concentrated
  8. customThe obtained residue was dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cb1794368b80459bb7439a7908378fb8
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07998656B2

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