反应详情

A solution of 2-(4-iodophenyl)-N-isobutoxycarbonyl-N-(3-methoxy-5-methylpyrazin-2-yl)pyridine-3-sulphonamide (1.5 g), methyl acrylate (0.25 ml), palladium acetate (58 mg) and triethylamine (1.79 ml) in dimethyl formamide (45 ml) and water (5 ml) was heated at 100° C. for 1 hour. Volatile material was removed by evaporation and water (50 ml) was added to the residue. The mixture was acidfied to pH 3 with 1M hydrochloric acid and extracted with ethyl acetate (2×50 ml). The extracts were washed with water (50 ml) and saturated sodium chloride solution (50 ml), treated with charcoal and dried (MgSO4). The solvent was removed by evaporation and the residue was triturated with ether/hexane (1:1 v/v) to give N-isobutoxycarbonyl-2-[4-(2-[methoxycarbonyl]vinyl)phenyl]-N-(3-methoxy-5-methylpyrazin-2-yl)pyridine-3-sulphonamide (0.99 g), m.p. 149-151° C.; microanalysis found: C, 57.7; H, 5.2; N, 10.6%; C26H28N407S requires: C, 57.8; H, 5.2; N, 10.4%.

1. customVolatile material was removed by evaporation and water (50 ml)
2. additionwas added to the residue
3. extractionextracted with ethyl acetate (2×50 ml)
4. washThe extracts were washed with water (50 ml) and saturated sodium chloride solution (50 ml)
5. additiontreated with charcoal
6. dry with materialdried (MgSO4)
7. customThe solvent was removed by evaporation
8. customthe residue was triturated with ether/hexane (1:1 v/v)