反应详情

温度

0 °C

A solution of the product of step (b), 1.38 g, 0.0050 moles, was dissolved in 20 ml of water. The solution was gradually treated with sodium carbonate, 0.84 g, 0.0100 moles, and cooled to 0° C. Next a solution of 0.5 ml of acetic anhydride in 10 ml of tetrahydrofuran was added. This was stirred overnight under nitrogen. The mixture was diluted with enough water to bring the volume to 100 ml. and washed with 20 ml of chloroform. The aqueous layer was made basic with 50% sodium hydroxide and extracted with 20 ml of chloroform (twice). The chloroform was dried with potassium carbonate, filtered and evaporated. The oil was dissolved in ml of isopropanol and treated with 1 ml of concentrated hydrochloric acid. This mix was then diluted to 250 ml with ether. The solids were filtered and washed with 10 ml of ether (twice). The sample was allowed to dry overnight to yield N-(3-((methylcarbonyl)amino)phenyl)-1-pyrrolidinecarboximidamide monohydrochloride. Yield: 350 mg, m.p. 193-196° C.

1. washand washed with 20 ml of chloroform
2. extractionextracted with 20 ml of chloroform (twice)
3. dry with materialThe chloroform was dried with potassium carbonate
4. filtrationfiltered
5. customevaporated
6. dissolutionThe oil was dissolved in ml of isopropanol
7. additiontreated with 1 ml of concentrated hydrochloric acid
8. additionThis mix was then diluted to 250 ml with ether
9. filtrationThe solids were filtered
10. washwashed with 10 ml of ether (twice)
11. customto dry overnight