Hydrazine hydrate (1:1) → Ammonia

HRID 419842

Reaktionsgleichung

Reaktionsgleichung von HRID 419842
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][CH2:8][C:9]([O:11]CC)=O.O.[NH2:15][NH2:16]>C(O)(C)C>[NH3:1].[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][CH2:8][C:9]([NH:15][NH2:16])=[O:11]

Komponenten

5

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 22396258Ethyl 2-pyrimidinyloxyacetate

Produkt 2

HCID 222AmmoniaHCID 593475352-(Pyrimidin-2-yloxy)acetohydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

A mixture of ethyl 2-pyrimidinyloxyacetate (GB2373186, step i ex 368) (4.4 g, 24.15 mmol) and hydrazine hydrate (5 mL, 160 mmol) in isopropanol (30 mL) was heated under reflux for 1 hour. The mixture was then cooled and concentrated under reduced pressure and the residue was purified by column chromatography on silica gel using dichloromethane:methanol:0.88 ammonia (100:0:0 to 100:10:1) to provide the title compound, 600 mg.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. temperatureThe mixture was then cooled
  4. concentrationconcentrated under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-18a1d1b403a64c7798710f754feaa548
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08093400B2

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