Reaktion #480547

Reaktionsgleichung

water

Ethyl N-hydroxyacetimidate

sodium hydride

2-Chloro-3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-6-trifluoromethyl-4(3H)-pyrimidinone

→

3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-2-[(1-ethoxyethylidene)aminooxy]-6-trifluoromethyl-4(3H)-pyrimidinone

Ausbeute 85.0%

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred at 0° C. for 3 hours
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   EinengenThe ethyl acetate solution was concentrated
4. 4
   Sonstigepurified by column chromatography on silica gel(20% ethyl acetate/hexane)
5. 5
   Sonstigeto give compound II-1 (0.90 g, yield 85%) as a white solid, m.p.152-155° C.

Vorschrift

Ethyl N-hydroxyacetimidate(0.23 g, 0.002 mol) was added dropwise to a suspension of sodium hydride(008 g, 0.002 mol) in tetrahydrofuran(5 ml) with stirring at 0° C. 2-Chloro-3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-6-trifluoromethyl-4(3H)-pyrimidinone(0.93 g, 0.002 mol) was added to the mixture at 0° C., and the mixture was stirred at 0° C. for 3 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The ethyl acetate solution was concentrated and purified by column chromatography on silica gel(20% ethyl acetate/hexane) to give compound II-1 (0.90 g, yield 85%) as a white solid, m.p.152-155° C.

Quelle