Реакция #710472

Уравнение реакции

chloroacetic acid

EDC-HCl

1-[(6-chloropyridin-3-yl)methyl]pyridin-2(1H)-imine hydrochloride

→

2-chloro-N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-acetamide

Выход 5.0%

Растворители

dichloromethane

dichloromethane

Условия реакции

Обработка

1. 1
   workup.ADDITIONto dilute the mixture
2. 2
   Промывкаthe mixture was washed with water
3. 3
   Сушкаa 1% HCl aqueous solution, dried over anhydrous magnesium sulfate
4. 4
   Концентрированиеconcentrated under reduced pressure
5. 5
   Другоеto obtain the subject material
6. 6
   ДругоеAmount obtained 4 mg (yield 5%)

Методика

70 mg (0.27 mmol) of the 1-[(6-chloropyridin-3-yl)methyl]pyridin-2(1H)-imine hydrochloride obtained by the method described in another method of Synthetic Example P1 was dissolved in 4 ml of anhydrous dichloromethane, 82 mg (0.67 mmol) of DMAP, 25 mg (0.27 mmol) of chloroacetic acid and 62 mg (0.32 mmol) of EDC-HCl were added thereto in sequence, and the resulting mixture was stirred at room temperature overnight. After the reaction was completed, dichloromethane was added thereto to dilute the mixture, and the mixture was washed with water and a 1% HCl aqueous solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain the subject material. Amount obtained 4 mg (yield 5%).

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