反应详情

10% Palladium on charcoal (0.5 g) was added to a solution of isobutyl 5-ethenyl-2-hydroxybenzoate (6.6 g, 30 mmol) and 4-iodo-N-(3-methyl-2-pyridinyl)benzenesulfonamide (11.2 g, 30 mmol) in dimethylacetamide (10 ml) and tributylamine (10 ml, 42 mmol) at 110° C. After 90 min. the solution was filtered and diluted with isopropanol (0.3 l) and chilled in a freezer. The product was filtered off, dried and dissolved in boiling formic acid (100 ml). The solution was filtered and water (65 ml) was added. After cooling to refrigerator temperature the product was filtered off and dried to yield 7.2g (51%) product.

1. filtrationAfter 90 min. the solution was filtered
2. additiondiluted with isopropanol (0.3 l)
3. temperaturechilled in a freezer
4. filtrationThe product was filtered off
5. customdried
6. dissolutiondissolved
7. filtrationThe solution was filtered
8. additionwater (65 ml) was added
9. temperatureAfter cooling to refrigerator temperature the product
10. filtrationwas filtered off
11. customdried