Reacción #1359752

Ecuación de reacción

tert-butyl chloride

lithium

2,6-difluoro-1-lithiobenzene

acetic anhydride

1,3-difluorobenzene

→

2,6-difluoroacetophenone

Rendimiento 92.0%

Disolventes

THF

THF

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroat −78° C
2. 2
   Temperaturahas been cooled to −5° C

Procedimiento

A solution of tert-butyllithium in THF is firstly produced by reacting 9.25 g of tert-butyl chloride with 1.4 g of lithium granules in 100 g of THF at −78° C. After a conversion of >97% (GC a/a) has been reached, 1,3-difluorobenzene (11.4 g) is added and the mixture is stirred for another 30 minutes at −78° C. and subsequently for 2 hours at −65° C. The resulting solution of 2,6-difluoro-1-lithiobenzene is added dropwise to a solution of 22 g of acetic anhydride in 35 g of THF which has been cooled to −5° C. After the usual aqueous work-up, 2,6-difluoroacetophenone is obtained in a yield of 92%.

Fuente