HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 3-Chloro-o-cresol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 2,6-Dichlorotoluene | HCID 8368 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | Dibenzo-18-crown-6 | HCID 26541 | — |
| Lösungsmittel | Diethylene Glycol | HCID 8117 | — |
| Produkt | 3-Chloro-o-cresol | HCID 14856 | — |
Reaktionsschritte
16.1 g (0.1 mol) of 2,6-dichlorotoluene, 19.8 g (0.3 mol) of potassium hydroxide (85%) and 0.3 g of dibenzo-18-crown-6 are heated in 30 ml of diethylene glycol at a bath temperature of 190° C. with reflux for 16 hours. The water released during the reaction is distilled off. After cooling, the reaction mixture is stirred with 100 ml of water until a solution is obtained and extracted three times with 50 ml of dichloromethane. The aqueous phase is admixed with 35 ml of 30% hydrochloric acid and extracted three times with 70 ml of dichloromethane. The organic phases are dried and concentrated under reduced pressure. 3-Chloro-2-methylphenol is obtained as a solid (11.5 g, content by HPLC: 97%, 78% of theory).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06756512B2 |
| Quelldatensatz | uspto-grants-2004_06 |
| ORD ID | ord-47cdf0d64c614343b118c960586e4a29 |
| Quellennotiz | uspto-grants-2004_06 |