Methane → Ethyl 4-(5-chloro-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinecarboxylate

HRID 2417794

Reaktionsgleichung

Reaktionsgleichung von HRID 2417794
[C:1]([N:6]1[CH2:11][CH2:10][CH:9]([NH:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[NH2:20])[CH2:8][CH2:7]1)([O:3][CH2:4][CH3:5])=[O:2].N[C:22](N)=[O:23].C>C1(C)C=CC=CC=1>[C:1]([N:6]1[CH2:7][CH2:8][CH:9]([N:12]2[C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[NH:20][C:22]2=[O:23])[CH2:10][CH2:11]1)([O:3][CH2:4][CH3:5])=[O:2]

Komponenten

5

Edukt 3

HCID 297MethaneHCID 1176UreaHCID 104609Ethyl 4-(2-amino-4-chloroanilino)piperidine-1-carboxylate

Produkt 1

HCID 104610Ethyl 4-(5-chloro-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinecarboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 24.7 g of 1-carbethoxy-4-(2-amino-4-chloroanilino)-piperidine and 7.2 g of urea was heated to 160°-180° C. for 3.5 hours. The melt was taken up in 250 ml of toluene and heated, while stirring, until everything had dissolved. The solution was clarified with active charcoal, filtered and concentrated to 50 ml. The product was precipitated with diisopropyl ether. Melting point: 160° C.

Aufarbeitung

  1. temperaturewas heated to 160°-180° C. for 3.5 hours
  2. temperatureheated
  3. dissolutionhad dissolved
  4. filtrationfiltered
  5. concentrationconcentrated to 50 ml
  6. customThe product was precipitated with diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-ce47b2e418934eda94a0f219f6f3ac23
Quelldatensatz
uspto-grants-1984_09
Patentnummer
US04470989

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