反応 #710477

反応方程式

water

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

triethylamine

trichloroacetyl chloride

water

→

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

収率 62.0%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   その他the reaction and liquid separation
2. 2
   洗浄The organic layer was washed once with water and twice with 1% hydrochloric acid
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   濃縮concentrated under reduced pressure
5. 5
   workup.ADDITIONDiethyl ether was added
6. 6
   その他to precipitate a solid
7. 7
   その他thus the solid was collected
8. 8
   その他dried
9. 9
   その他to obtain the subject material
10. 10
    その他Amount obtained 61 mg (yield 62%)

実験手順

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, 94 μl (0.68 mmol, 68 mg) of triethylamine and 33 g (0.27 mmol, 49 mg) of trichloroacetyl chloride were added thereto in sequence, and the resulting mixture was stirred at room temperature for 1 hour. After the reaction was completed, water was added thereto to stop the reaction and liquid separation was performed with dichloromethane and water. The organic layer was washed once with water and twice with 1% hydrochloric acid, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. Diethyl ether was added thereto to precipitate a solid, and thus the solid was collected and dried to obtain the subject material. Amount obtained 61 mg (yield 62%).

出典