Reacción #710477

Ecuación de reacción

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

Rendimiento 62.0%

Disolventes

dichloromethane

dichloromethane

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe reaction and liquid separation
2. 2
   LavadoThe organic layer was washed once with water and twice with 1% hydrochloric acid
3. 3
   Secadodried over anhydrous magnesium sulfate
4. 4
   Concentraciónconcentrated under reduced pressure
5. 5
   workup.ADDITIONDiethyl ether was added
6. 6
   Otroto precipitate a solid
7. 7
   Otrothus the solid was collected
8. 8
   Otrodried
9. 9
   Otroto obtain the subject material
10. 10
    OtroAmount obtained 61 mg (yield 62%)

Procedimiento

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%).

Fuente