反应详情

A mixture of 8.7 g. of 4-[(2,4-diamino-5-pyrimidinyl)-methyl]-2,6-dimethoxy-carbanilic acid ethyl ester and 1.44 g. of sodium hydride (50% dispersion in oil) in 75 ml. of absolute dimethylformamide was stirred at room temperature for 1 hour and then treated with 4.26 g. of methyl iodide. After stirring at room temperature for 3 hours, the dimethylformamide was removed at 60° C. under vacuum. The residue was dissolved in a mixture of 500 ml. of ethyl acetate and 150 ml. of water. After separation of the phases, the aqueous phase was extracted with 500 ml. of ethyl acetate. The combined ethyl acetate extracts were washed with 300 ml. of water, dried over magnesium sulfate and evaporated under vacuum. After recrystallization of the residue from alcohol, there was obtained 4-[(2,4-diamino-5-pyrimidinyl)-methyl]-2,6-dimethoxy-N-methyl-carbanilic acid ethyl ester having a melting point of 187°-188° C.

1. additionA mixture of 8.7 g
2. additiontreated with 4.26 g
3. customthe dimethylformamide was removed at 60° C. under vacuum
4. dissolutionThe residue was dissolved in a mixture of 500 ml
5. customAfter separation of the phases
6. extractionthe aqueous phase was extracted with 500 ml
7. washThe combined ethyl acetate extracts were washed with 300 ml
8. dry with materialof water, dried over magnesium sulfate
9. customevaporated under vacuum
10. customAfter recrystallization of the residue from alcohol