تفاعل #65369

معادلة التفاعل

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

p-t-butyl-benzene sulphonamide potassium

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

المردود 93.0%

المذيبات

dimethyl sulphoxide

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر