반응 #62710

반응 방정식

sodium carbonate

3-aminobenzotrifluoride

1-chloro-2,3-propanediol

→

2,3-dihydroxypropyl-3-aminobenzotrifluoride

용매

ethoxyethanol

반응 조건

후처리

1. 1
   온도refluxing condenser
2. 2
   온도While this mixture was cooling
3. 3
   기타the temperature below 35° C
4. 4
   온도The mixture was then heated
5. 5
   온도to reflux for 24 hours
6. 6
   기타Afterwards, the crude reaction mixture
7. 7
   여과was filtered from the salt by-product
8. 8
   세척The salt was then washed several times with chloroform
9. 9
   기타The solvent and chloroform was then removed under low vacuum and high vacuum

실험 절차

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.

출처