Reaktion #70655

ord-bb3372ca47a9425ba89b4ac18a1052b0

Reaktionsgleichung

O
water
NNc1ccc2[nH]c(=O)c(-c3ccccc3)cc2n1
6-hydrazino-3-phenyl-1,5-naphthyridin-2(1H)-one
CCOC(=O)C(F)F
ethyl difluoroacetate
O=C(O)C(F)F
difluoroacetic acid
O=c1[nH]c2ccc3nnc(C(F)F)n3c2cc1-c1ccccc1
1-(difluoromethyl)-8-phenyl[1,2,4]triazolo[4,3-a]-1,5-naphthyridin-7(6H)-one

Lösungsmittel

Reaktionsbedingungen

Temperatur
200°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe resulting solid was collected by filtration

Vorschrift

A mixture of 6-hydrazino-3-phenyl-1,5-naphthyridin-2(1H)-one (7-2) (21 g, 83 mmol), ethyl difluoroacetate (31 g, 250 mmol), and difluoroacetic acid (200 mg, 2.08 mmol) in DMI (100 mL) was heated under microwave irradiation at 200° C. for 1 h. To the cooled mixture was added water, and the resulting solid was collected by filtration to give 1-(difluoromethyl)-8-phenyl[1,2,4]triazolo[4,3-a]-1,5-naphthyridin-7(6H)-one (10-1) as pale yellow solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536193B2uspto-grants-2013_09