Triphenylphosphine → HCID 86651838, Verbindung

HRID 1465446Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1465446
[Cl:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH:12][NH:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])=[O:11])=[CH:5][CH:4]=1.[C:21]1([P:27]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C1C=CC=CC=1>[Cl-:1].[C:17]([O:16][C:14]([NH:13][NH:12][C:10]([CH2:9][C:6]1[CH:7]=[CH:8][C:3]([CH2:2][P+:27]([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)=[CH:4][CH:5]=1)=[O:11])=[O:15])([CH3:20])([CH3:19])[CH3:18]

Komponenten

4

Edukt 2

HCID 11776TriphenylphosphineHCID 67266620HCID 67266620, Verbindung

Produkt 1

HCID 86651838HCID 86651838, VerbindungAusbeute 78,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A mixture of tert-butyl 2-{[4-(chloromethyl)phenyl]acetyl}hydrazinecarboxylate (5.9 g, 19.7 mmol), triphenylphosphine (5.18 g, 19.7 mmol) and benzene (15 ml) was heated under reflux for 21 hrs. After cooling to room temperature, the precipitate was collected by filtration, washed 3 times with benzene, and dried under reduced pressure to give {4-[2-(tert-butoxycarbonyl)hydrazinocarbonylmethyl]benzyl}(triphenyl)phosphonium chloride (8.68 g, yield 78%) as a white solid.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 21 hrs
  3. filtrationthe precipitate was collected by filtration
  4. washwashed 3 times with benzene
  5. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d805eba4b89d4119a13c71d88d8163c5
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US08999989B2

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