反応 #62710

反応方程式

sodium carbonate

3-aminobenzotrifluoride

1-chloro-2,3-propanediol

→

2,3-dihydroxypropyl-3-aminobenzotrifluoride

溶媒

ethoxyethanol

反応条件

後処理

1. 1
   温度refluxing condenser
2. 2
   温度While this mixture was cooling
3. 3
   その他the temperature below 35° C
4. 4
   温度The mixture was then heated
5. 5
   温度to reflux for 24 hours
6. 6
   その他Afterwards, the crude reaction mixture
7. 7
   ろ過was filtered from the salt by-product
8. 8
   洗浄The salt was then washed several times with chloroform
9. 9
   その他The solvent and chloroform was then removed under low vacuum and high vacuum

実験手順

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.

出典