Reacción #710493

Ecuación de reacción

water

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

methyl iodide

potassium hydroxide

→

desired product

Rendimiento 39.0%

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

Rendimiento 39.0%

Disolventes

dimethoxyethane

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaAfter cooling
2. 2
   Extracciónwas extracted twice with 150 mL of ethyl acetate
3. 3
   LavadoThe organic phase was washed twice with 100 mL of water
4. 4
   Secadodried over magnesium sulfate
5. 5
   Concentraciónconcentrated
6. 6
   OtroAfter purification on silica

Procedimiento

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.

Fuente