反应详情

温度

40 °C

To a mixture of 286 g (2 mole) of 3-methyl-4-chlorophenol, 700 ml of tertiary butanol, 700 ml of water and 3.0 mole of 1,4-dichloro-2-butanol, sodium hydroxide (2.9 moles, 230 g in 700 ml of water) was added with stirring at 40° C. to maintain a pH of 9.5-10.0 as the reaction progressed. The addition was 10 hr; the reaction was stirred at 40° C. for 48 hr. The resulting reaction mixture was extracted with chloroform sodium hydroxide at 25° C. The chloroform extract was washed with sodium sulfate. The dried chloroform solution was concentrated and the residue was distilled under reduced pressure to give 110.9 g of the product which distilled at 135°-143° C./0.007 mm and melted at 87°-89° C. after recrystallization with isopropanol and petroleum ether (30°-60° C.).

1. additionwas added
2. temperatureto maintain a pH of 9.5-10.0 as the reaction
3. additionThe addition
4. stirringthe reaction was stirred at 40° C. for 48 hr
5. customThe resulting reaction mixture
6. extractionwas extracted with chloroform sodium hydroxide at 25° C
7. extractionThe chloroform extract
8. washwas washed with sodium sulfate
9. concentrationThe dried chloroform solution was concentrated
10. distillationthe residue was distilled under reduced pressure