反应 #710477

反应方程式

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

收率 62.0%

溶剂

dichloromethane

dichloromethane

反应条件

后处理

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

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, 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%).

来源