反应详情

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).

1. temperaturewith reflux for 16 hours
2. distillationis distilled off
3. temperatureAfter cooling
4. customis obtained
5. extractionextracted three times with 50 ml of dichloromethane
6. extractionextracted three times with 70 ml of dichloromethane
7. customThe organic phases are dried
8. concentrationconcentrated under reduced pressure