Реакция #700980

Уравнение реакции

isoprene

4-chloro-1-methyl-4,5,5-trifluorocyclohexene

5-chloro-1-methyl-4,4,5-trifluorocyclohexene

chlorotrifluoroethylene

→

3,4-difluorotoluene

Условия реакции

Обработка

1. 1
   ДругоеAs shown in the above reaction
2. 2
   Другоеis prepared
3. 3
   Другоеat temperature range of 390 to 480° C.
4. 4
   Другоеthrough continuous vapor phase condensation in a flow reactor
5. 5
   workup.DISTILLATIONdistilling the resultant

Методика

As shown in the above reaction, a mixture of 4-chloro-1-methyl-4,5,5-trifluorocyclohexene (IIIa) and 5-chloro-1-methyl-4,4,5-trifluorocyclohexene (IIIb) is prepared by reacting chlorotrifluoroethylene (CTFE) (I) and isoprene (II) at temperature range of 390 to 480° C. through continuous vapor phase condensation in a flow reactor and distilling the resultant. The mixture is dehydrohalogenated in the presence of alkali metal hydroxide and a phase transition catalyst to form 3,4-difluorotoluene (IV). The 3,4-difluorotoluene is reacted with chlorine gas in the presence of catalysts consisting of ferro-shaving and ferric chloride at temperature range of -10 to 40° C. without using any organic solvent to form 2-chloro-4,5-difluorotoluene (V). The 2-chloro-4,5-difluorotoluene is photo-reacted with chlorine gas under a lighting mercury lamp at temperature range of 80 to 140° C. without using any organic solvent to form 2-chloro-4,5-difluorobenzotrichloride (VI). The 2-chloro-4,5-difluorobenzotrichloride is reacted with aqueous acid solution at temperature range of 35 to 80° C. without using any organic solvent to give 2-chloro-4,5-difluorobenzoic acid (VII). The 2-chloro-4,5-difluorobenzoyl chloride (VIII) according to the present invention is prepared by reacting 2-chloro-4,5-difluorobenzotrichloride (VI) with zinc oxide.

Источник