Reaktion #2045090

ord-98e68468bdc6461aa7fd5638d4378afa

Reaktionsgleichung

NN.O
Hydrazine hydrate
CC1(O)OC(=O)C(c2c(F)cccc2Cl)=C1c1ccc(Cl)nc1
3-(2-chloro-6-fluoro-phenyl)-4-(6-chloro-pyridin-3-yl)-5-hydroxy-5-methyl-5H-furan-2-one
COC(C)(C)C
tert-butyl methyl ether
Cc1n[nH]c(=O)c(-c2c(F)cccc2Cl)c1-c1ccc(Cl)nc1
4-(2-chloro-6-fluoro-phenyl)-5-(6-chloro-pyridin-3-yl)-6-methyl-2H-pyridazin-3-one

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthis mixture is heated for 7 h to 120° C
  2. 2
    Filtrationfiltered
  3. 3
    WaschenThe solid remainder is washed with tert-butyl methyl ether

Vorschrift

Hydrazine hydrate (12 g) is added to a solution of 3-(2-chloro-6-fluoro-phenyl)-4-(6-chloro-pyridin-3-yl)-5-hydroxy-5-methyl-5H-furan-2-one (Compound No. II.a.1, 80 g) in 400 ml of 1-butanol and this mixture is heated for 7 h to 120° C. Subsequently, the mixture is poured into 400 ml of tert-butyl methyl ether. The resulting mixture is stirred for 30 min, then cooled to 0° C. and filtered. The solid remainder is washed with tert-butyl methyl ether to deliver 4-(2-chloro-6-fluoro-phenyl)-5-(6-chloro-pyridin-3-yl)-6-methyl-2H-pyridazin-3-one (Compound No. I.a.01) as colourless solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08410026B2uspto-grants-2013_04