Reaktion #710997

Reaktionsgleichung

NaH

2-chloro-6-trifluoromethylisonicotinonitrile

IPA

→

yellow oil

Ausbeute 71.8%

2-isopropoxy-6-(trifluoromethyl)isonicotinonitrile

Ausbeute 71.8%

Lösungsmittel

THF

—

ice water

ethyl acetate

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAt 0° C
2. 2
   SonstigeAt 0° C
3. 3
   TemperaturMaintained 0° C. temperature for 30 min
4. 4
   SonstigeCompletion of reaction
5. 5
   SonstigeReaction mixture
6. 6
   WaschenOrganic layer was washed by water two times
7. 7
   Trocknendried over Na2SO4
8. 8
   Filtrationfiltered
9. 9
   Einengenconcentrated by rotary evaporation (40° C., 20 mmHg)

Vorschrift

In a 250-ml capacity 3 neck flask (1.39 g) NaH suspended in 100 ml THF. At 0° C. IPA (4.36 g) in 20 ml THF added in this reaction flask. Allow it to stir at RT for 3 h. At 0° C. 2-chloro-6-trifluoromethylisonicotinonitrile (10 g) in 80 mL THF added in the flask in dropwise manner. Maintained 0° C. temperature for 30 min. Completion of reaction conformed by TLC. Reaction mixture was dumped in ice water. Extract compound in ethyl acetate. Organic layer was washed by water two times & dried over Na2SO4, filtered, and concentrated by rotary evaporation (40° C., 20 mmHg) to afford 8 g of yellow oil. The resulting crude compound forwarded for next step.

Quelle