反应详情

A mixture of 2-iodobenzoic acid (14.9 g, 0.06 mol), 5-amino-1,3-dimethylpyrazole (6.7 g, 0.06 mol), DMF (125 ml), Cu(OAc)2 (0,4 g) and K2CO3 (8.28 g, 0.06 mol) was refluxed overnight. The reaction mixture was poured into ice-water (500 ml) and then was acidified with acetic acid to a pH of about 5. The solid which formed was collected by filtration, washed with water (100 ml) and dried. The solid was dissolved in hot CHCl3 (300 ml), filtered, dried over MgSO4 and evaporated to about 20 ml. Hexane (50 ml) was added and then the product was collected by filtration, washed with hexane (30 ml) and dried to afford 6.2 g of N-(1,3-dimethyl-pyrazol-5-yl)anthranilic acid, m.p. 210-211° C.

1. temperaturewas refluxed overnight
2. customThe solid which formed
3. filtrationwas collected by filtration
4. washwashed with water (100 ml)
5. customdried
6. dissolutionThe solid was dissolved in hot CHCl3 (300 ml)
7. filtrationfiltered
8. dry with materialdried over MgSO4
9. customevaporated to about 20 ml
10. additionHexane (50 ml) was added
11. filtrationthe product was collected by filtration
12. washwashed with hexane (30 ml)
13. customdried