Реакция #710493

Уравнение реакции

water

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

methyl iodide

potassium hydroxide

→

desired product

Выход 39.0%

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

Выход 39.0%

Растворители

dimethoxyethane

Условия реакции

Обработка

1. 1
   ТемператураAfter cooling
2. 2
   Экстракцияwas extracted twice with 150 mL of ethyl acetate
3. 3
   ПромывкаThe organic phase was washed twice with 100 mL of water
4. 4
   Сушкаdried over magnesium sulfate
5. 5
   Концентрированиеconcentrated
6. 6
   ДругоеAfter purification on silica

Методика

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.

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