Reacción #65369

Ecuación de reacción

4-[4-chloro-5-(2-chloro-5-methoxy-phenoxy)-6-methyl-pyrimidin-2-yl]-morpholine

p-t-butyl-benzene sulphonamide potassium

→

4-tert-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-methyl-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide

Rendimiento 93.0%

Disolventes

dimethyl sulphoxide

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.DISTILLATIONThereafter, the dimethylsulphoxide was distilled off
2. 2
   Otrothe residue was partitioned between ethyl acetate and 1N hydrochloric acid
3. 3
   Lavadothe organic phase was washed neutral
4. 4
   OtroThe organic phase was dried
5. 5
   Otrothe solvent was evaporated
6. 6
   Otrothe residue was recrystallized from dichloromethane-ethanol

Procedimiento

10.7 g of 4-[4-chloro-5-(2-chloro-5-methoxy-phenoxy)-6-methyl-pyrimidin-2-yl]-morpholine and 21.6g of p-t-butyl-benzene sulphonamide potassium in 150 ml of dry dimethyl sulphoxide were heated to 120° C. under argon for 16 hours. Thereafter, the dimethylsulphoxide was distilled off, the residue was partitioned between ethyl acetate and 1N hydrochloric acid and the organic phase was washed neutral. The organic phase was dried, the solvent was evaporated and the residue was recrystallized from dichloromethane-ethanol. There were obtained 14.7 g 4-tert-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-methyl-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide, m.p 154° C., MS: M=546.

Fuente