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Trifluoroacetic acid → HCID 9888078, Verbindung

HRID 723326
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 723326
CO[CH:3](OC)[CH2:4][N:5]([C:21]1[CH:26]=[CH:25][C:24](OC2C=CC=CC=2)=[CH:23][CH:22]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][N:18]([CH3:20])[CH3:19])=[CH:11][CH:10]=1)=[O:7].F[C:37](F)(F)[C:38]([OH:40])=O>>[CH3:19][N:18]([CH3:20])[CH2:17][CH2:16][O:15][C:12]1[CH:11]=[CH:10][C:9]([N:8]2[CH:3]=[CH:4][N:5]([C:21]3[CH:26]=[CH:25][C:24]([O:40][C:38]4[CH:37]=[CH:11][CH:10]=[CH:9][CH:14]=4)=[CH:23][CH:22]=3)[C:6]2=[O:7])=[CH:14][CH:13]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 6422Trifluoroacetic acidHCID 21873333HCID 21873333, Verbindung

Produkt 1

HCID 9888078HCID 9888078, Verbindung

Versuchsvorschrift

1-(2,2-Dimethoxyethyl)-3-[4-(2-dimethylaminoethoxy)phenyl]-1-(4-phenoxy-phenyl)urea (0.33 g) was shaken with trifluoroacetic acid (5 ml) for 16 hours. Volatiles were removed and the residue was taken up in dichloromethane (10 ml) and washed with sodium hydroxide solution (0.1N; 1 ml). The aqueous phase was extracted with dichloromethane (10 ml), and the combined organic phases were concentrated. The residue was purified by chromatography on silica gel (eluent: dichloromethane/methanol 98:2 with 1% v/v 7N ammonia solution in methanol). The product with the molecular weight of 415.50 (C25H25N3O3); MS (ESI): 416 ([M+H]+), was obtained in this way.

Aufarbeitung

  1. customVolatiles were removed
  2. washwashed with sodium hydroxide solution (0.1N; 1 ml)
  • extractionThe aqueous phase was extracted with dichloromethane (10 ml)
  • concentrationthe combined organic phases were concentrated
  • customThe residue was purified by chromatography on silica gel (eluent
  • customMS (ESI): 416 ([M+H]+), was obtained in this way
  • Quellen und Nachweise

    ORD-Eintrag
    ord-bde9c62aaa9d46c4b3f850ce716c244d
    Quelldatensatz
    uspto-grants-2006_11
    DOI
    10.6084/m9.figshare.5104873.v1
    Patentnummer
    US07141561B2

    Notizen zur Reaktion

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