Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Chloroacetic Acid | HCID 300 | — |
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 3,4-Dichlorobenzyl chloride | HCID 7609 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Thiourea | HCID 2723790 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 178526174 | HCID 178526174 | 89,3% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US04225617 |
|---|
| Quelldatensatz | uspto-grants-1980_09 |
|---|
| ORD ID | ord-82f0ccebe0c344529afcf12476748e39 |
|---|
| Quellennotiz | uspto-grants-1980_09 |
|---|