Reaktion #55079

Reaktionsgleichung

sodium carbonate

NaOH

chloroacetic acid

HCl

3,4-dichlorobenzylchloride

thiourea

→

stated product

Ausbeute 89.3%

3,4-Dichlorobenzylthioacetic acid

Ausbeute 89.3%

Lösungsmittel

water

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturare heated
2. 2
   Temperaturunder reflux for 30 minutes
3. 3
   Sonstigeis run in at 60°-70° C.
4. 4
   Temperaturthe mixture is heated
5. 5
   Temperaturunder reflux for 15 minutes
6. 6
   Sonstigeis run in at 60°-70° C.
7. 7
   Temperaturthe mixture is maintained
8. 8
   Temperaturunder reflux for 1 hour
9. 9
   Extraktionextracted with ether
10. 10
    Waschenthe extract is washed with water
11. 11
    Sonstigedried
12. 12
    Sonstigeevaporated
13. 13
    Filtrationfiltered off

Vorschrift

A mixture of 19.5 g (0.1 mol) of 3,4-dichlorobenzylchloride and 7.6 g (0.1 mol) of thiourea in 50 ml of water are heated under reflux for 30 minutes with stirring, and then a solution of 16 g (0.4 mol) of NaOH in 25 ml of water is run in at 60°-70° C.; the mixture is heated under reflux for 15 minutes, a solution of 15 g (0.15 mol) of chloroacetic acid, 7 g of sodium carbonate and 50 ml of water is run in at 60°-70° C., and the mixture is maintained under reflux for 1 hour. The mixture is acidified cold with concentrated HCl, extracted with ether, and the extract is washed with water, dried and evaporated. The residue is taken up in petroleum ether and filtered off. 21 g of the stated product are obtained (yield: 83%) melting point: 63°-64° C.

Quelle