반응 #710477

반응 방정식

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

수율 62.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   기타the reaction and liquid separation
2. 2
   세척The organic layer was washed once with water and twice with 1% hydrochloric acid
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   농축concentrated under reduced pressure
5. 5
   workup.ADDITIONDiethyl ether was added
6. 6
   기타to precipitate a solid
7. 7
   기타thus the solid was collected
8. 8
   기타dried
9. 9
   기타to obtain the subject material
10. 10
    기타Amount obtained 61 mg (yield 62%)

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, 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%).

출처