반응 #710493

반응 방정식

water

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

methyl iodide

potassium hydroxide

→

desired product

수율 39.0%

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

수율 39.0%

용매

dimethoxyethane

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   추출was extracted twice with 150 mL of ethyl acetate
3. 3
   세척The organic phase was washed twice with 100 mL of water
4. 4
   건조dried over magnesium sulfate
5. 5
   농축concentrated
6. 6
   기타After purification on silica

실험 절차

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.

출처