Reaktion #455598

Reaktionsgleichung

ethyl 3-ethoxy-2-(3-chloro-2,4,5-trifluorobenzoyl)acrylate

ethyl 3-chloro-2,4,5-trifluorobenzoylacetate

2-amino-3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridine

→

title compound

ethyl 8-chloro-1-[3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridine-2-yl]-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe solution was concentrated under reduced pressure
2. 2
   workup.ADDITIONto the residue were added 1.3 g of anhydrous potassium carbonate and 3 ml of N,N-dimethylformamide
3. 3
   Temperaturto cool
4. 4
   SonstigeThe solution was separated
5. 5
   workup.ADDITIONby adding 30 ml of chloroform and 300 ml of distilled water
6. 6
   Waschenthe chloroform layer was washed twice with 300 ml of distilled water
7. 7
   Trocknendried over anhydrous magnesium sulfate
8. 8
   Einengenconcentrated under reduced pressure

Vorschrift

To 3 ml chloroform solution of ethyl 3-ethoxy-2-(3-chloro-2,4,5-trifluorobenzoyl)acrylate prepared from 0.78 g of ethyl 3-chloro-2,4,5-trifluorobenzoylacetate by normal process was added 0.90 g of 2-amino-3,5-difluoro-6-(p-methoxybenzylamino)-4-methylpyridine. The solution was concentrated under reduced pressure, and to the residue were added 1.3 g of anhydrous potassium carbonate and 3 ml of N,N-dimethylformamide, and the mixture was stirred at 90° C. for 15 minutes and allowed to cool. The solution was separated by adding 30 ml of chloroform and 300 ml of distilled water, and the chloroform layer was washed twice with 300 ml of distilled water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain the title compound as a brown crude oil.

Quelle