Reaktion #1269835

ord-9d02b594518149c18cc301409a75f635

Reaktionsgleichung

O
water
COC(=C(C#N)C#N)c1ccc(Oc2ccccc2)cc1
1,1-Dicyano-2-methoxy-2-(4-phenoxyphenyl)ethene
COC(=C(C#N)C#N)c1ccc(Oc2ccccc2)cc1
1,1-dicyano-2-methoxy-2-(4-phenoxyphenyl)ethene
NN.O
hydrazine hydrate
N#Cc1c(N)n[nH]c1-c1ccc(Oc2ccccc2)cc1
3-amino-4-cyano-5-(4-phenoxyphenyl)pyrazole

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated on the steambath for 1 hour
  2. 2
    SonstigeThe precipitated solid is collected
  3. 3
    Waschenwashed with ethanol:water (4:1)
  4. 4
    Sonstigedried in air

Vorschrift

1,1-Dicyano-2-methoxy-2-(4-phenoxyphenyl)ethene (22.5 g) and 1,1-dicyano-2-methoxy-2-(4-phenoxyphenyl)ethene oil (15 g) are treated with a solution of hydrazine hydrate (18 mL) in ethanol (25 mL) and heated on the steambath for 1 hour. Ethanol (15 mL) is added followed by water (10 mL). The precipitated solid is collected and washed with ethanol:water (4:1) and then dried in air to give 3-amino-4-cyano-5-(4-phenoxyphenyl)pyrazole as a pale orange solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08663961B2uspto-grants-2014_03