Dimethylformamide → HCID 898498, Verbindung

HRID 1084825Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1084825
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([OH:15])=[O:14])=[O:9].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[CH2:31](I)[CH3:32]>CC(C)=O>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([O:15][CH2:31][CH3:32])=[O:14])=[O:9]

Komponenten

6

Edukt 4

HCID 6228Dimethylformamide2×HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 3063368HCID 3063368, Verbindung

Produkt 1

HCID 898498HCID 898498, VerbindungAusbeute 65,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a suspension of 2-[3-(2-thienyl)acrylamido]benzoic acid (273 mg, 1 mmol) in acetone (2 ml) were added potassium carbonate (194 mg, 1.4 mmol) and dry dimethylformamide (1 ml). To the resulting solution, ethyl iodide (218 mg, 1.4 mmol) and dry dimethylformamide (2 ml) were added and the mixture was stirred at 60° C. for 1 hour. The reaction mixture was poured into ice water. The precipitated solid was collected by suction, and recrystallized from methanol to give pale yellow crystals of the desired compound (197 mg, yield, 65%). m.p., 120°-122° C.

Aufarbeitung

  1. customThe precipitated solid was collected by suction
  2. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-51c3f0397e8f469bb8be3e0dffc61165
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05006548

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