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Ammonium hexafluorophosphate → 3-Benzyl-1-methoxy-4,5-dimethylimidazolium hexafluorophosphate

HRID 1984956
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1984956
[I-].[CH2:2]([N:9]1[C:13]([CH3:14])=[C:12]([CH3:15])[N+:11]([O:16][CH3:17])=[CH:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[F:18][P-:19]([F:24])([F:23])([F:22])([F:21])[F:20].[NH4+]>O>[F:18][P-:19]([F:24])([F:23])([F:22])([F:21])[F:20].[CH2:2]([N:9]1[C:13]([CH3:14])=[C:12]([CH3:15])[N+:11]([O:16][CH3:17])=[CH:10]1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 9793912Ammonium hexafluorophosphateHCID 178502610HCID 178502610, Verbindung

Produkt 1

HCID 1785026093-Benzyl-1-methoxy-4,5-dimethylimidazolium hexafluorophosphate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

Crude iodide 2 was taken up in deionized (DI) water, which separated the product from small amounts of a dark, insoluble residue. The water solution was decanted to a second flask and a solution of ammonium hexafluorophosphate (950 mg, ca. 5.8 mmol) in 10 mL of DI water was added in portions. An oil separated during the addition, and the supernatant solution was decanted out. The oil was crushed in cold (0° C.), and subsequently recrystallized in methanol. Yield: 1.3 g (73% from 1). 1H-NMR (δ, CDCl3): 8.67 (s, 1H, N—CH—N); 7.39 (m, 3H, C6H5); 7.29 (d, 2H, C6H5); 5.24 (s, 2H, NCH2); 4.21 (s, 3H, OCH3); 2.27 (s, 3H, CH3); 2.17 (s, 3H, CH3).

Aufarbeitung

  1. customseparated the product from small amounts of a dark, insoluble residue
  2. customThe water solution was decanted to a second flask
  3. customAn oil separated during the addition
  4. customthe supernatant solution was decanted out
  5. customThe oil was crushed in cold (0° C.)
  6. customsubsequently recrystallized in methanol

Quellen und Nachweise

ORD-Eintrag
ord-7e4c833eced74f94ac4ecc1c5232ee3f
Quelldatensatz
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07544800B2

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