反应详情

Acetonitrile (20 ml), followed by N,N-diisopropylethylamine (5.8 ml, 33 mmol) were added to 2,4-dimethyl-3-pyridinecarboxylic acid (5.1 g, 33 mmol). The mixture was stirred for 5 minutes, then 2-chloromethyl-4-isopropyl-6-methoxysaccharin (4.3 g, 14 mmol) was added. The reaction mixture was stirred at room temperature for 47 hours, then at 80° C. for 1 hour. The mixture was diluted with ethyl acetate (100 ml), washed with saturated NaHCO3, and the organic layer was dried over Na2SO4. The solvent was removed in vacuo and the residue was recrystallized from ether to afford 3,4 g (57%) of 4-isopropyl-6-methoxy-2-saccharinylmethyl 2,4-dimethylpyridine-3 carboxylate, m.p. 132.1°-133.5° C.

1. stirringThe reaction mixture was stirred at room temperature for 47 hours
2. waitat 80° C. for 1 hour
3. washwashed with saturated NaHCO3
4. dry with materialthe organic layer was dried over Na2SO4
5. customThe solvent was removed in vacuo
6. customthe residue was recrystallized from ether