反应详情

温度

100 °C

A mixture of methyl 7-(2-bromo-4-fluorobenzenesulfonylamino)-4H-furo[2,3-c]chromene-6-carboxylate (Intermediate 10, 2.04 g), N,N-diethyl-N—((Z)-1-tributylstannanylprop-1-en-3-yl)amine (Intermediate 11, 3.4 g), tri-tert-butylphosphonium tetrafluoroborate (0.246 g), tris-(dibenzylideneacetone)dipalladium (0.0.388 g) in dioxane (35 mL) was degassed and purged with argon then heated at 100° C. for 3.5 hours. After cooling, the mixture was diluted with ethyl acetate and filtered. The filtrate was washed with water, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of ammonia in methanol (2M) and DCM with a gradient of 0-10%. The product was triturated with ether and the solid was collected by filtration to give methyl 7-[2-((Z)-3-diethylaminoprop-1-en-1-yl)-4-fluorobenzenesulfonyl-amino]-4H-furo[2,3-c]chromene-6-carboxylate (1.47 g) as a pale orange solid.

1. customwas degassed
2. custompurged with argon
3. temperatureAfter cooling
4. additionthe mixture was diluted with ethyl acetate
5. filtrationfiltered
6. washThe filtrate was washed with water
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customThe filtrate was evaporated to dryness
10. customthe residue was purified by chromatography on silica
11. washeluting with a mixture of ammonia in methanol (2M) and DCM with a gradient of 0-10%
12. customThe product was triturated with ether
13. filtrationthe solid was collected by filtration