反応 #710493

反応方程式

water

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

methyl iodide

potassium hydroxide

→

desired product

収率 39.0%

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

収率 39.0%

溶媒

dimethoxyethane

反応条件

後処理

1. 1
   温度After cooling
2. 2
   抽出was extracted twice with 150 mL of ethyl acetate
3. 3
   洗浄The organic phase was washed twice with 100 mL of water
4. 4
   乾燥dried over magnesium sulfate
5. 5
   濃縮concentrated
6. 6
   その他After purification on silica

実験手順

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.

出典