تفاعل #710472

معادلة التفاعل

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

المردود 5.0%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONto dilute the mixture
2. 2
   غسيلthe mixture was washed with water
3. 3
   تجفيفa 1% HCl aqueous solution, dried over anhydrous magnesium sulfate
4. 4
   تركيزconcentrated under reduced pressure
5. 5
   أخرىto obtain the subject material
6. 6
   أخرىAmount obtained 4 mg (yield 5%)

الإجراء التجريبي

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%).

المصدر