Hydrazine hydrate (1:1) → 4-Hydrazinyl-6-(piperidin-1-yl)pyrimidine

HRID 876656Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 876656
O.[NH2:2][NH2:3].Cl[C:5]1[CH:10]=[C:9]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[N:8]=[CH:7][N:6]=1>C(O)C>[NH:2]([C:5]1[CH:10]=[C:9]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[N:8]=[CH:7][N:6]=1)[NH2:3]

Komponenten

4

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

17.7 ml (18.2 g, 364.2 mmol) hydrazine hydrate are added dropwise to a solution of 6.0 g (30.4 mmol) 4-chloro-6-piperidin-1-ylpyrimidine in 50 ml ethanol at RT, while stiffing. The reaction solution is subsequently stirred at 80° C. for 16 h. For working up, the mixture is concentrated in vacuo, the residue is stirred in water, the solid which has precipitated out is filtered off, the residue on the filter is washed twice with 150 ml water each time and twice with 100 ml diethyl ether each time and the product is dried in vacuo.

Aufarbeitung

  1. concentrationthe mixture is concentrated in vacuo
  2. stirringthe residue is stirred in water
  3. customthe solid which has precipitated out
  4. filtrationis filtered off
  5. washthe residue on the filter is washed twice with 150 ml water each time
  6. dry with materialtwice with 100 ml diethyl ether each time and the product is dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3a09ba6981e249eca5b56922820a7c3a
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08987261B2

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