Ethyl 2-oxocyclohexanecarboxylate → HCID 178517489, Verbindung

HRID 1824719

Reaktionsgleichung

Reaktionsgleichung von HRID 1824719
O=[C:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[C:8]([O:10]CC)=O.Cl.[Cl:14][C:15]1[CH:23]=[CH:22][C:18]([C:19]([NH2:21])=[NH:20])=[CH:17][CH:16]=1.CC([O-])(C)C.[K+]>CO>[Cl:14][C:15]1[CH:23]=[CH:22][C:18]([C:19]2[N:21]=[C:8]([OH:10])[C:3]3[CH2:4][CH2:5][CH2:6][CH2:7][C:2]=3[N:20]=2)=[CH:17][CH:16]=1

Komponenten

5

Edukt 3

HCID 95543Ethyl 2-oxocyclohexanecarboxylateHCID 2034364-Chlorobenzene-1-carboximidamide hydrochlorideHCID 23665647Potassium tert-butoxide

Produkt 1

HCID 178517489HCID 178517489, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

7.5 g of ethyl 2-oxocyclohexane-1-carboxylate and 9.6 g of 4-chlorobenzamidine hydrochloride were introduced into 50 ml of methanol. 5.6 g of potassium tert-butylate were added with stirring. The reaction mixture was stirred under reflux for 4 hours and then poured onto ice water. The crystalline product was filtered off with suction, washed with water and recrystallized from dimethylformamide. Yield: 8.8 g; m.p.: >300° C.

Aufarbeitung

  1. stirringThe reaction mixture was stirred
  2. temperatureunder reflux for 4 hours
  3. additionpoured onto ice water
  4. filtrationThe crystalline product was filtered off with suction
  5. washwashed with water
  6. customrecrystallized from dimethylformamide

Quellen und Nachweise

ORD-Eintrag
ord-181f678d553d4d9bbbc10bdca3367880
Quelldatensatz
uspto-grants-2006_05
Patentnummer
US07045526B2

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