Triethylamine → HCID 14624371, Verbindung

HRID 1650765

Reaktionsgleichung

Reaktionsgleichung von HRID 1650765
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][N:11]=[C:12](Br)[C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15].[CH2:21]([N:23]([CH2:26][CH3:27])[C:24]#[N:25])[CH3:22].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:21]([N:23]([C:24]1[N:10]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][C:4]=2[Cl:9])[N:11]=[C:12]([C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15])[N:25]=1)[CH2:26][CH3:27])[CH3:22]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 12050DiethylcyanamideHCID 86743923HCID 86743923, Verbindung

Produkt 1

HCID 14624371HCID 14624371, VerbindungAusbeute 54,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

3.4 g (0.008 mol) of pentafluoropropionyl bromide 2,4,6-trichlorophenylhydrazone and 0.8 g (0.008 mol) of N,N-diethylcyanamide were added to 20 ml of toluene. Then, 0.9 g (0.009 mol) of triethylamine was added thereto under stirring at room temperature. After completion of the dropwise addition, stirring was continued at room temperature for further 1 hour. Then, 20 ml of toluene was added thereto, followed by washing with water. The organic layer was dried, and the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 1.9 g (yield: 54.3%) of the desired compound as a brown powder. Melting point: 66°-70° C.

Aufarbeitung

  1. additionAfter completion of the dropwise addition
  2. stirringstirring
  3. washby washing with water
  4. customThe organic layer was dried
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-4dab9342e66f404f853b7217f76fd96a
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04925864

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