Reacción #62710

Ecuación de reacción

sodium carbonate

3-aminobenzotrifluoride

1-chloro-2,3-propanediol

→

2,3-dihydroxypropyl-3-aminobenzotrifluoride

Disolventes

ethoxyethanol

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturarefluxing condenser
2. 2
   TemperaturaWhile this mixture was cooling
3. 3
   Otrothe temperature below 35° C
4. 4
   TemperaturaThe mixture was then heated
5. 5
   Temperaturato reflux for 24 hours
6. 6
   OtroAfterwards, the crude reaction mixture
7. 7
   Filtraciónwas filtered from the salt by-product
8. 8
   LavadoThe salt was then washed several times with chloroform
9. 9
   OtroThe solvent and chloroform was then removed under low vacuum and high vacuum

Procedimiento

In a two liter three necked flask equipped with mechanical stirrer, refluxing condenser and thermometer was added 322.2 gms (2.0 moles) of 3-aminobenzotrifluoride, 500 ml of ethoxyethanol solvent and 442.0 gms (4 moles) 1-chloro-2,3-propanediol. While this mixture was cooling, 205 gms (2.36 moles) of sodium carbonate was added keeping the temperature below 35° C. The mixture was then heated to reflux for 24 hours. Afterwards, the crude reaction mixture was filtered from the salt by-product. The salt was then washed several times with chloroform and these washings were combined with the filtrate. The solvent and chloroform was then removed under low vacuum and high vacuum to give 450.5 gms of the crude bis-2,3-dihydroxypropyl-3-aminobenzotrifluoride as a viscous dark oil.

Fuente