تفاعل #56465

معادلة التفاعل

1,1,2-trichlorobutadiene

water

triethylamine

isobutyric acid dimethylamide

→

1,1,2-trichlorobutadiene

dimethylamine

المذيبات

methylene chloride

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىprepared
2. 2
   درجة الحرارةwhile cooling
3. 3
   درجة الحرارةthe mixture was then heated
4. 4
   درجة الحرارةrefluxed for 1 hour
5. 5
   درجة الحرارةAfter heating
6. 6
   درجة الحرارةunder reflux for 5 hours
7. 7
   workup.STIRRINGthe mixture was stirred overnight (15 hours)
8. 8
   أخرىSeparating the phases
9. 9
   تجفيفdrying the organic phase over sodium sulphate
10. 10
    workup.DISTILLATIONto fractional distillation

الإجراء التجريبي

50.0 g (0.5 mol) of triethylamine in 100 ml of methylene chloride was added dropwise to 350 ml of the solution, prepared according to Example 7a, of the amide chloride of isobutyric acid dimethylamide in methylene chloride at 20° C., while cooling and stirring, and the mixture was then heated and refluxed for 1 hour. Thereafter, 75.0 g (0.55 mol) of zinc chloride were added at 10° C. and 79.0 g (0.5 mol) of 1,1,2-trichlorobutadiene were added dropwise to the reaction solution in the course of 60 minutes. After heating under reflux for 5 hours, 400 ml of water were added to the reaction solution and the mixture was stirred overnight (15 hours). Separating the phases and drying the organic phase over sodium sulphate and subjecting it to fractional distillation gave 10.5 g of 1,1,2-trichlorobutadiene, 11.5 g of isobutryic acid dimethylamine and 66.8 g (59%, relative to isobutyric acid dimethylamine employed) of the ketone of boiling point 112°-117° C./10 mm Hg and refractive index nD20 of 1.509.

المصدر