反応 #710466

反応方程式

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

EDC-HCl

dibromoacetic acid

→

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

収率 15.0%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   洗浄washed once with water and twice with a 1% HCl aqueous solution
2. 2
   乾燥dried over anhydrous magnesium sulfate
3. 3
   濃縮concentrated under reduced pressure
4. 4
   その他to obtain the subject material
5. 5
   その他Amount obtained 50 mg (yield 15%)

実験手順

200 mg (0.78 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, 238 mg (1.95 mmol) of DMAP and 224 mg (1.17 mmol) of EDC-HCl were dissolved in 10 ml of anhydrous dichloromethane, 101 μl (202 mg, 1.17 mmol) of dibromoacetic acid was added thereto, and the resulting mixture was stirred at room temperature overnight. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed once with water and twice with a 1% HCl aqueous solution, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain the subject material. Amount obtained 50 mg (yield 15%)

出典