Hydrazine hydrate (1:1) → HCID 178451811, Verbindung

HRID 1888207Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1888207
[Br:1][C:2]1[CH:3]=[C:4]([C:24]#[N:25])[C:5](F)=[C:6]([C:8]([CH:10]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]2)=O)[CH:7]=1.O.[NH2:27][NH2:28]>C(O)C>[Br:1][C:2]1[CH:7]=[C:6]2[C:5](=[C:4]([C:24]#[N:25])[CH:3]=1)[NH:28][N:27]=[C:8]2[CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 59022871HCID 59022871, Verbindung

Produkt 1

HCID 178451811HCID 178451811, VerbindungAusbeute 59 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 1,1-dimethylethyl 4-[(5-bromo-3-cyano-2-fluorophenyl)carbonyl]-1-piperidinecarboxylate (1.35 g, 3.3 mmols) and hydrazine hydrate (0.21 ml, 6.9 mmols) in ethanol (30 mL) was heated at reflux overnight. After cooling, the solvent was evaporated and the residue was purified by flash chromatography eluting with pentane/ethyl acetate 4:1 v/v to give the title compound (0.78 g) as a yellow solid (59%).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. temperatureAfter cooling
  4. customthe solvent was evaporated
  5. customthe residue was purified by flash chromatography
  6. washeluting with pentane/ethyl acetate 4:1 v/v

Quellen und Nachweise

ORD-Eintrag
ord-df771e4b77904824b85a5327e4120681
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08501780B2

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