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Hydrochloric Acid → Triethylammonium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propane-1-sulfonate

HRID 252899
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 252899
[CH2:1]([N:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2].Cl.[F:9][C:10]([F:27])([S:23]([O-:26])(=[O:25])=[O:24])[CH:11]([O:16][C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[C:12]([F:15])([F:14])[F:13].[Na+].ClCCl>O.C(OCC)C>[F:27][C:10]([F:9])([S:23]([O-:26])(=[O:24])=[O:25])[CH:11]([O:16][C:17](=[O:22])[C:18]([CH3:20])([CH3:21])[CH3:19])[C:12]([F:13])([F:15])[F:14].[CH2:1]([NH+:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2]
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Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 8471TriethylamineHCID 86616368Sodium 1,1,3,3,3-Pentafluoro-2-(pivaloyloxy)propane-1-sulfonate

Produkt 1

HCID 86618175Triethylammonium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propane-1-sulfonateAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

Triethylamine was dissolved in cold water, and hydrochloric acid was added thereto to adjust the pH of the reaction liquid to fall within a range of 1 to 3. Then sodium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate and dichloromethane were added thereto and stirred. The separated organic layer was washed with water, and dichloromethane was removed under reduced pressure from the washed organic layer. To the residue thus obtained, diethyl ether was added for recrystallization. The resultant was filtrated and dried to obtain a desired product at a yield of 75%. The structure of the obtained product was identified using 1H-NMR, IR and TOFMS spectra.

Aufarbeitung

  1. customthe pH of the reaction liquid
  2. washThe separated organic layer was washed with water, and dichloromethane
  3. customwas removed under reduced pressure from the washed organic layer
  4. customTo the residue thus obtained
  5. filtrationThe resultant was filtrated
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9d821aab383c42b985c8a0ba3e1b29df
Quelldatensatz
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07871761B2

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