反应详情

Iodine monochloride (5.103 g) was added dropwise to a stirred solution of 1-(4-amino-3-methylphenyl)-1,2,4-triazole (5.22 g) and sodium acetate (2.583 g) in acetic acid (100 cm3). After 16 hours volatile material was removed in vacuo and the residue was partitioned between dichloromethane (100 cm3) and sodium carbonate solution (50 cm3). The organic phase was washed with sodium thiosulphate solution (10 g in 50 cm3 water), dried (MgSO4) and evaporated to give a solid which was chromatographed on silica (Merck "MK 60.9385" [Trade Mark]) eluting with ethyl acetate. Combination and evaporaton of the appropriate fractions gave a solid which was recrystallised from ethyl acetate-ether to afford the title compound, m.p. 151°-154° (3.1 g).

1. customAfter 16 hours volatile material was removed in vacuo
2. customthe residue was partitioned between dichloromethane (100 cm3) and sodium carbonate solution (50 cm3)
3. washThe organic phase was washed with sodium thiosulphate solution (10 g in 50 cm3 water)
4. dry with materialdried (MgSO4)
5. customevaporated
6. customto give a solid which
7. customwas chromatographed on silica (Merck "MK 60.9385" [Trade Mark])
8. washeluting with ethyl acetate
9. customCombination and evaporaton of the appropriate fractions gave a solid which
10. customwas recrystallised from ethyl acetate-ether