반응 #710472

반응 방정식

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

수율 5.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONto dilute the mixture
2. 2
   세척the mixture was washed with water
3. 3
   건조a 1% HCl aqueous solution, dried over anhydrous magnesium sulfate
4. 4
   농축concentrated under reduced pressure
5. 5
   기타to obtain the subject material
6. 6
   기타Amount obtained 4 mg (yield 5%)

실험 절차

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%).

출처