Реакция #65369

Уравнение реакции

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

Выход 93.0%

Растворители

dimethyl sulphoxide

Условия реакции

Обработка

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

Методика

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.

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