Reaktion #65369

Reaktionsgleichung

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

Ausbeute 93.0%

Lösungsmittel

dimethyl sulphoxide

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle