반응 #92968

반응 방정식

1,4-dichloro-2-butanol

sodium hydroxide

3-methyl-4-chlorophenol

tertiary butanol

→

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

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONTo a mixture of 286 g
2. 2
   온도to 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
   기타The resulting reaction mixture
6. 6
   추출was extracted with chloroform sodium hydroxide at 25° C
7. 7
   추출The chloroform extract
8. 8
   세척was washed with sodium sulfate
9. 9
   농축The dried chloroform solution was concentrated
10. 10
    workup.DISTILLATIONthe residue was distilled under reduced pressure
11. 11
    기타to give 110.9 g
12. 12
    workup.DISTILLATIONof the product which distilled at 135°-143° C./0.007 mm
13. 13
    기타and melted at 87°-89° C. after recrystallization with isopropanol and pet. ether (30.60°)

실험 절차

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°).

출처