反应 #710472

反应方程式

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

收率 5.0%

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   workup.ADDITIONto dilute the mixture
2. 2
   洗涤the mixture was washed with water
3. 3
   干燥a 1% HCl aqueous solution, dried over anhydrous magnesium sulfate
4. 4
   浓缩concentrated under reduced pressure
5. 5
   其他to obtain the subject material
6. 6
   其他Amount obtained 4 mg (yield 5%)

实验过程

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%).

来源