Reacción #1361997

Ecuación de reacción

hydrochloric acid

4-dimethylamino-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide

2,2,3,3,3-pentafluoropropionaldehyde monohydrate

benzene

→

aimed product

4-dimethylamino-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2,3,3,3-pentafluoropropylidene] hydrazide

Disolventes

water

ethyl acetate

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe obtained mixture was refluxed
2. 2
   OtroThe obtained reaction solution
3. 3
   Otrothe organic phase separated from the solution
4. 4
   Lavadowas washed with saturated brine
5. 5
   Secadodried with anhydrous sodium sulfate
6. 6
   Concentraciónconcentrated
7. 7
   OtroThe obtained concentrated solution was purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)

Procedimiento

4-dimethylamino-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide (0.30 g, 0.00088 mol) was mixed with 2,2,3,3,3-pentafluoropropionaldehyde monohydrate (0.29 g, 0.00088×2.0 mol) and benzene, and further with a small amount of concentrated hydrochloric acid. The obtained mixture was refluxed and dehydrated for about 8 hours using a water separator. The obtained reaction solution was distributed in ethyl acetate-saturated sodium bicarbonate water, and the organic phase separated from the solution was washed with saturated brine, dried with anhydrous sodium sulfate and then concentrated. The obtained concentrated solution was purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

Fuente