Diethyl Ether → HCID 178506551, Verbindung

HRID 2378712Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2378712
[I-:1].[NH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH2:11][N+](C)(C)C)=[N:3]1.[C:16]1([P:22]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(OCC)C>CN(C=O)C>[I-:1].[NH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH2:11][P+:22]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)=[N:3]1

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 11776TriphenylphosphineHCID 178483384HCID 178483384, Verbindung

Produkt 1

HCID 178506551HCID 178506551, VerbindungAusbeute 92,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

(1H-indazol-3-ylmethyl)trimethylammonium iodide (45.0 g, 142 mmol) obtained in Step 3 was dissolved in DMF (220 mL), and the solution was mixed with triphenylphosphine (44.7 g, 170 mmol), followed by heating under reflux for 2.5 hours. After cooling to room temperature, the reaction mixture was added with diethyl ether and was stirred overnight. The resulting precipitates were collected by filtration to obtain (1H-indazol-3-ylmethyl)triphenylphosphonium iodide (68.3 g, 92%).

Aufarbeitung

  1. temperatureby heating
  2. temperatureunder reflux for 2.5 hours
  3. customThe resulting precipitates
  4. filtrationwere collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-b24b19a4a87b4131b527251f6cf9cd43
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07470717B2

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