Triethylamine → HCID 14624341, Verbindung

HRID 1650764

Reaktionsgleichung

Reaktionsgleichung von HRID 1650764
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:6][C:5]=1[NH:14][N:15]=[C:16](Br)[C:17]([CH3:20])([CH3:19])[CH3:18])([O-:3])=[O:2].[CH2:22]([N:24]([CH2:27][CH3:28])[C:25]#[N:26])[CH3:23].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:22]([N:24]([C:25]1[N:14]([C:5]2[CH:6]=[CH:7][C:8]([C:10]([F:13])([F:12])[F:11])=[CH:9][C:4]=2[N+:1]([O-:3])=[O:2])[N:15]=[C:16]([C:17]([CH3:20])([CH3:19])[CH3:18])[N:26]=1)[CH2:27][CH3:28])[CH3:23]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 12050DiethylcyanamideHCID 86743922HCID 86743922, Verbindung

Produkt 1

HCID 14624341HCID 14624341, VerbindungAusbeute 84,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

7.4 g (0.02 mol) of 2,2-dimethylpropionyl bromide 2-nitro-4-trifluoromethylphenylhydrazone and 2.0 g (0.02 mol) of N,N-diethylcyanamide were added to 100 ml of toluene. Then, 2.2 g (0.022 mol) of triethylamine was dropwise added under stirring at room temperature. After completion of the dropwise addition, stirring was continued at room temperature for further 1 hour. Then, 100 ml of toluene was added and washed with water. The organic layer was dried, and the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 6.5 g (yield: 84.4%) of the desired compound as a pale yellow liquid. Refractive index nD20 : 1.4911.

Aufarbeitung

  1. additionAfter completion of the dropwise addition
  2. stirringstirring
  3. washwashed 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-4eb6eb4f9ae149d9bf2610c10b131d30
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04925864

Verknüpfte Notizen

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