反应详情

温度

0 °C

A solution of the product of Example 1, 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. A solution of 2-chlorobenzoyl chloride, 0.96 g, 0.0053 moles, in 10 ml of tetrahydrofuran was added. This mixture was allowed to stir over the weekend. The mixture was then diluted with water to 100 ml and washed with 20 ml of chloroform. The mixture 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 by vacuum evaporation. The residue was taken up in 20 ml of isopropanol, treated with 1 ml of concentrated hydrochloric acid, and then diluted to 250 ml with ether. The solid that precipitated was collected by filtration and washed with 10 ml of ether (twice). The solid was then recrystallized with methanol and ether and dried in the vacuum oven to provide N-(3-(((2-chlorophenyl)carbonyl)amino)phenyl)-1-pyrrolidinecarboximidamide monohydrochloride. Yield: 1.1 g, m.p. 145° C. (dec)

1. washwashed 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 by vacuum evaporation
6. additiontreated with 1 ml of concentrated hydrochloric acid
7. additiondiluted to 250 ml with ether
8. customThe solid that precipitated
9. filtrationwas collected by filtration
10. washwashed with 10 ml of ether (twice)
11. customThe solid was then recrystallized with methanol and ether
12. customdried in the vacuum oven