反应 #710493

反应方程式

water

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

methyl iodide

potassium hydroxide

→

desired product

收率 39.0%

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

收率 39.0%

溶剂

dimethoxyethane

反应条件

后处理

1. 1
   温度After cooling
2. 2
   萃取was extracted twice with 150 mL of ethyl acetate
3. 3
   洗涤The organic phase was washed twice with 100 mL of water
4. 4
   干燥dried over magnesium sulfate
5. 5
   浓缩concentrated
6. 6
   其他After purification on silica

实验过程

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.

来源