تفاعل #92968

معادلة التفاعل

1,4-dichloro-2-butanol

sodium hydroxide

3-methyl-4-chlorophenol

tertiary butanol

→

4-Chloro-1-(4-chloro-3-methylphenoxy)-2-butanol

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONTo a mixture of 286 g
2. 2
   درجة الحرارةto maintain a pH of 9.5-10.0 as the reaction
3. 3
   workup.ADDITIONThe addition
4. 4
   workup.STIRRINGthe reaction was stirred at 40° C. for 48 hr
5. 5
   أخرىThe resulting reaction mixture
6. 6
   استخلاصwas extracted with chloroform sodium hydroxide at 25° C
7. 7
   استخلاصThe chloroform extract
8. 8
   غسيلwas washed with sodium sulfate
9. 9
   تركيزThe dried chloroform solution was concentrated
10. 10
    workup.DISTILLATIONthe residue was distilled under reduced pressure
11. 11
    أخرىto give 110.9 g
12. 12
    workup.DISTILLATIONof the product which distilled at 135°-143° C./0.007 mm
13. 13
    أخرىand melted at 87°-89° C. after recrystallization with isopropanol and pet. ether (30.60°)

الإجراء التجريبي

To a mixture of 286 g. (2 moles) of 3-methyl-4-chlorophenol, 700 ml. of tertiary butanol, 700 ml. of water and 3.0 moles of 1,4-dichloro-2-butanol, sodium hydroxide (2.9 moles, 230 g. in 700 ml. 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 pet. ether (30.60°).

المصدر