4-Fluorophenyl isocyanate → HCID 70288795, Verbindung

HRID 1290783Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1290783
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][NH:19][CH2:20][CH:21]([O:24][CH3:25])[O:22][CH3:23])[CH2:13][CH2:12]3)[C:5]=2[O:4][CH2:3][CH2:2]1.[F:26][C:27]1[CH:32]=[CH:31][C:30]([N:33]=[C:34]=[O:35])=[CH:29][CH:28]=1>C(Cl)Cl>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][N:19]([CH2:20][CH:21]([O:22][CH3:23])[O:24][CH3:25])[C:34]([NH:33][C:30]4[CH:31]=[CH:32][C:27]([F:26])=[CH:28][CH:29]=4)=[O:35])[CH2:13][CH2:12]3)[C:5]=2[O:4][CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 709554-Fluorophenyl isocyanateHCID 702900421-(1,4-Benzodioxan-5-yl)-4-(2-(2,2-dimethoxy-1-ethylamino)-1-ethyl)piperazine

Produkt 1

HCID 70288795HCID 70288795, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 1-(1,4-benzodioxan-5-yl)-4-(2-(2,2-dimethoxy-1-ethylamino)-1-ethyl)piperazine (2.3 g) and 4-fluorophenyl isocyanate (0.9 g) in methylene chloride (100 ml) was refluxed for 2 h. Removal of solvent in vacuo gave an oil which was purified on a silica gel column (eluent: ethyl acetate/methanol=3:1). The product, 1-(1,4-benzodioxan5-yl)-4-(2-(N-(2,2-dimethoxy 1-ethyl)-N-(4-fluorophenylaminocarbonyl)-amino)-1-ethyl)piperazine, was obtained as a solid (2.5 g).

Aufarbeitung

  1. customRemoval of solvent in vacuo
  2. customgave an oil which
  3. customwas purified on a silica gel column (eluent: ethyl acetate/methanol=3:1)

Quellen und Nachweise

ORD-Eintrag
ord-3a8a88867dc0414e879c751a7a712a07
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05753661

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