Hydrazine hydrate (1:1) → 1-(Pyridin-2-yl)piperidine-4-carbohydrazide

HRID 269734Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 269734
C([O:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)[CH2:8][CH2:7]1)=O)C.O.[NH2:19][NH2:20]>CO>[N:9]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)[CH2:10][CH2:11][CH:6]([C:4]([NH:19][NH2:20])=[O:3])[CH2:7][CH2:8]1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)2×HCID 38156184-Piperidinecarboxylic acid, 1-(2-pyridinyl)-, ethyl ester

Produkt 1

HCID 235440481-(Pyridin-2-yl)piperidine-4-carbohydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

3,4,5,6-Tetrahydro-2H-[1,2′]bipyridinyl-4-carboxylic acid ethyl ester (35 g, 150 mmol) (see reference Farmaco, 1993, 48(10), 1439) was dissolved in methanol (700 mL) containing hydrazine hydrate (34 mL, 150 mmol) and was heated under reflux for 18 hours. After this time, more hydrazine hydrate (22.7 mL, 100 mmol) was added and the mixture stirred for a further 18 hours. The mixture was cooled to room temperature and evaporated under reduced pressure. The solid formed was triturated with ethyl acetate to give the title compound as a white solid.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. customevaporated under reduced pressure
  4. customThe solid formed
  5. customwas triturated with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-91b6afd42fe54328a546719c646703e3
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07449462B2

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