反应详情

温度

120 °C

3,3-dimethylbutane-1-sulphonic acid amide potassium salt (616 mg) was added to a solution of 4,6-dichloro-5-(2-methoxyphenoxy)-2-(pyrimidin-2-yl)-pyrimidine (Can. Pat. Appl. 2071193) (353 mg) in dry dimethyl sulphoxide (10 ml) and the resulting mixture stirred at 120° C. for 6 hours under nitrogen. The reaction mixture was allowed to cool and then partitioned between ethyl acetate (30 ml ) and 2N aqueous hydrochloric acid (30 ml ) and the organic phase separated. The aqueous was extracted with ethyl acetate (30 ml) and the organic phases combined, washed (water 2×20 ml), dried (Na2SO4) and evaporated under reduced pressure. Column chromatography on silica eluting with a solvent gradient of pentane:ethyl acetate 50:50 changing to 0:100 and finally ethyl acetate:methanol 98:2 gave N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-3,3-dimethyl-1-butanesulfonamide as an off-white solid (440 mg).

1. temperatureto cool
2. custompartitioned between ethyl acetate (30 ml ) and 2N aqueous hydrochloric acid (30 ml )
3. customthe organic phase separated
4. extractionThe aqueous was extracted with ethyl acetate (30 ml)
5. washwashed (water 2×20 ml)
6. dry with materialdried (Na2SO4)
7. customevaporated under reduced pressure