تفاعل #710493

معادلة التفاعل

water

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

methyl iodide

potassium hydroxide

→

desired product

المردود 39.0%

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

المردود 39.0%

المذيبات

dimethoxyethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   استخلاصwas extracted twice with 150 mL of ethyl acetate
3. 3
   غسيلThe organic phase was washed twice with 100 mL of water
4. 4
   تجفيفdried over magnesium sulfate
5. 5
   تركيزconcentrated
6. 6
   أخرىAfter purification on silica

الإجراء التجريبي

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.

المصدر