반응 #65369

반응 방정식

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

수율 93.0%

용매

dimethyl sulphoxide

반응 조건

후처리

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

실험 절차

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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