Chloroform → HCID 178432502, Verbindung

HRID 1455305Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1455305
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)([NH2:12])[CH:9]([NH2:11])[CH3:10])=[CH:4][CH:3]=1.CO[C:22]([C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([C:30]#N)[CH:25]=1)=[NH:23].C(Cl)(Cl)Cl>CO>[C:22]([C:24]1[CH:25]=[C:26]([C:30]2[NH:11][CH:9]([CH3:10])[C:8]([C:13]3[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=3)([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)[N:12]=2)[CH:27]=[CH:28][CH:29]=1)#[N:23]

Komponenten

5

Edukt 3

HCID 6212ChloroformHCID 218859191,1-Bis(4-fluorophenyl)-1,2-propanediamineHCID 552656943-Cyano-benzimidic acid methyl ester

Produkt 1

HCID 178432502HCID 178432502, VerbindungAusbeute 14 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

1,1-bis(4-fluorophenyl)-1,2-propanediamine (50 mg) was dissolved in methanol (1 mL), and to the solution was added 3-cyanobenzeneimidic acid methyl ester (75 mg). The mixture was stirred at room temperature for 24 hrs. After chloroform (5 ml) was added to the reaction mixture, insolubles were removed by filtration. After concentrating the filtrate in vacuo, the obtained residue was purified by silica gel column chromatography (C-300; hexane: ethyl acetate=3:1→1:1) to give the objective compound (10 mg).

Aufarbeitung

  1. customwere removed by filtration
  2. concentrationAfter concentrating the filtrate in vacuo
  3. customthe obtained residue was purified by silica gel column chromatography (C-300; hexane: ethyl acetate=3:1→1:1)

Quellen und Nachweise

ORD-Eintrag
ord-002a05c7a5334da0a514b9167aa45dae
Quelldatensatz
uspto-grants-2009_01
Patentnummer
US07482358B2

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