Reaktion #710493

Reaktionsgleichung

water

1-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]acetone

methyl iodide

potassium hydroxide

→

desired product

Ausbeute 39.0%

3-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]butan-2-one

Ausbeute 39.0%

Lösungsmittel

dimethoxyethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   Extraktionwas extracted twice with 150 mL of ethyl acetate
3. 3
   WaschenThe organic phase was washed twice with 100 mL of water
4. 4
   Trocknendried over magnesium sulfate
5. 5
   Einengenconcentrated
6. 6
   SonstigeAfter purification on silica

Vorschrift

6.00 g of 1-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]acetone (Int-11) (27 mMol) (synthesis according to P10 and comm av.) and 5.75 g of methyl iodide (40.5 mMol) were diluted in 120 mL of dimethoxyethane. 3.03 g of potassium hydroxide were added portionwise at room temperature. After cooling, 100 mL of water were added to the reaction mixture which was extracted twice with 150 mL of ethyl acetate. The organic phase was washed twice with 100 mL of water, dried over magnesium sulfate and concentrated. After purification on silica, 0.67 g (39%) of desired product 3-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]butan-2-one (Int-12) were obtained, [M+1]=252.

Quelle