Triphenylsulfonium chloride → 912290-04-1

HRID 1404878

Reaktionsgleichung

Reaktionsgleichung von HRID 1404878
[Na].[F:2][C:3]([F:23])([S:19]([OH:22])(=[O:21])=[O:20])[C:4]([O:6][CH2:7][C:8]12[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][C:10]([OH:18])([CH2:11]3)[CH2:9]1)[CH2:15]2)=[O:5].[Cl-].[C:25]1([S+:31]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(Cl)(Cl)Cl>[OH:18][C:10]12[CH2:16][CH:14]3[CH2:13][CH:12]([CH2:17][C:8]([CH2:7][O:6][C:4]([C:3]([F:23])([F:2])[S:19]([O-:22])(=[O:20])=[O:21])=[O:5])([CH2:15]3)[CH2:9]1)[CH2:11]2.[C:38]1([S+:31]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1

Komponenten

5

Edukt 3

HCID 61343Triphenylsulfonium chlorideHCID 5360545SodiumHCID 577603663-Hydroxy-1-adamantylmethyl difluorosulfoacetate

Produkt 1

HCID 75607088912290-04-1

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a obtained solution of the sodium salt of 3-hydroxy-1-adamantylmethyl difluorosulfoacetate, 17.2 parts of chloroform, and 2.9 parts of a 14.8 mass % aqueous triphenyl sulfonium chloride solution were added, and the mixture was stirred for 15 hours, and then an organic layer was separated from the resultant solution, and an aqueous layer was subjected to extraction with 6.5 parts of chloroform. Organic layers were combined and washed with an ion-exchanged water, and the obtained organic layer was concentrated. To the concentrated solution, 5.0 parts of tert-butyl methyl ether was added, and the resultant mixture was stirred and filtered to obtain, as a white solid, 0.2 parts of triphenylsulfonium 1-((3-hydroxy-1-adamantyl)methoxycarbonyl)difluoromethane sulfonate (B1-2).

Aufarbeitung

  1. customan organic layer was separated from the resultant solution
  2. extractionan aqueous layer was subjected to extraction with 6.5 parts of chloroform
  3. washwashed with an ion-exchanged water
  4. concentrationthe obtained organic layer was concentrated
  5. additionTo the concentrated solution, 5.0 parts of tert-butyl methyl ether was added
  6. stirringthe resultant mixture was stirred
  7. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-6352577f1c45465290f2269cd7033acd
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08916330B2

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