反应详情

Methyl 2-(((n-propylamino)sulfonyl)amino)-3-pyridinecarboxylate (15.7 grams; 0.057 mole), 95 ml of water and 10.5 ml of 50 percent aqueous sodium hydroxide were mixed and the resulting reaction mixture stirred for about 11/4 hours at ambient temperatures. The reaction mixture was extracted with two -- 50 ml portions of methylene chloride and one -- 50 ml portion of ether to remove impurities. The aqueous layer was separated from the organic layer and acidified to a pH of about 4.5 with concentrated hydrochloric acid. The solution was filtered and the filtrate acidified to a pH of about 1. The resulting product precipitate was recovered by filtration, dissolved in acetone and the solution filtered and dried with magnesium sulfate. The mixture was again filtered and the filtrate reduced in vacuo to obtain the title compound as a yellow powder having a melting point of 208° C.-210° C.

1. customthe resulting reaction mixture
2. extractionThe reaction mixture was extracted with two
3. custom50 ml portions of methylene chloride and one -- 50 ml portion of ether to remove impurities
4. customThe aqueous layer was separated from the organic layer
5. filtrationThe solution was filtered
6. filtrationThe resulting product precipitate was recovered by filtration
7. dissolutiondissolved in acetone
8. filtrationthe solution filtered
9. dry with materialdried with magnesium sulfate
10. filtrationThe mixture was again filtered