反应详情

温度

150 °C

A mixture of phenol (87.5 g, 0.93 moles), xylene (100 ml), and zirconium tetrachloride (6.0 g, 0.026 moles) was heated to reflux under a slow nitrogen stream. The xylene was distilled through a 10 inch Vigreux column. The distillation was continued over a 2 hour period until the reaction mixture reached 177° C. Approximately 10 g of phenol was distilled with the xylene. The reaction mass was cooled to 150° C., and ethyl disulfide (62.0 g, 0.50 moles) was added. The reaction mixture was heated to 152° C., then heated slowly over a 5 hour period to 180° C., and finally held at 180° C. for an additional 10 hours. Ethyl mercaptan was removed continuously by distillation. The reaction mixture was cooled to 100° C., then vacuum distilled at 100 mm mercury until the pot temperature reached 200° C. to give 70.8 g of distillate. GC analysis indicated the distillate contained 34.0 g of ortho-(ethylthio)phenol (44% yield).

1. temperaturewas heated
2. temperatureto reflux under a slow nitrogen stream
3. distillationThe xylene was distilled through a 10 inch Vigreux column
4. distillationThe distillation
5. customreached 177° C
6. distillationApproximately 10 g of phenol was distilled with the xylene
7. temperatureThe reaction mixture was heated to 152° C.
8. temperatureheated slowly over a 5 hour period to 180° C.
9. waitfinally held at 180° C. for an additional 10 hours
10. customEthyl mercaptan was removed continuously by distillation
11. temperatureThe reaction mixture was cooled to 100° C.
12. distillationvacuum distilled at 100 mm mercury until the pot temperature
13. customreached 200° C.
14. customto give 70.8 g of distillate