Sodium Hydroxide → 5-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one

HRID 2417795

Reaktionsgleichung

Reaktionsgleichung von HRID 2417795
C([N:6]1[CH2:11][CH2:10][CH:9]([N:12]2[C:16]3[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:15]=3[NH:14][C:13]2=[O:22])[CH2:8][CH2:7]1)(OCC)=O.[OH-].[Na+].[Cl-].[NH4+]>O>[Cl:21][C:19]1[CH:18]=[CH:17][C:16]2[N:12]([CH:9]3[CH2:8][CH2:7][NH:6][CH2:11][CH2:10]3)[C:13](=[O:22])[NH:14][C:15]=2[CH:20]=1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 104610Ethyl 4-(5-chloro-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinecarboxylate

Produkt 1

HCID 1046075-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 22.3 g of 1-carbethoxy-4-(5-chlorobenzimidazol-2-on-1-yl)-piperidine, 13 g of 50% strength sodium hydroxide solution and 90 ml of water was boiled under reflux for 24 hours. After the mixture had been cooled, the solution was stirred with 8.5 g of ammonium chloride for 30 minutes and extracted with chloroform, and the undissolved material was filtered off and discarded. The chloroform solution was dried and evaporated. The product crystallized, and has a melting point of 220° C.

Aufarbeitung

  1. temperatureunder reflux for 24 hours
  2. temperatureAfter the mixture had been cooled
  3. extractionextracted with chloroform
  4. filtrationthe undissolved material was filtered off
  5. dry with materialThe chloroform solution was dried
  6. customevaporated
  7. customThe product crystallized

Quellen und Nachweise

ORD-Eintrag
ord-81f7d53e494e42f0a6b69705f54f78bd
Quelldatensatz
uspto-grants-1984_09
Patentnummer
US04470989

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