反应详情

Methyl 7-[2-((Z)-3-diethylaminoprop-1-enyl)-4-fluorobenzenesulfonylamino]-4H-furo[2,3-c]chromene-6-carboxylate (Intermediate 9, 0.129 g) was added to a solution of lithium hydroxide monohydrate (0.42 g) in water (2 mL) and dioxane (8 mL), and the mixture was irradiated in the microwave at 130° C. for 1 hour. After cooling, the mixture was acidified with formic acid, and evaporated to dryness. The residue was triturated with 10% methanol in DCM, filtered and the filtrate was evaporated to dryness. The residue was purified by chromatography on silica, eluting with a mixture of methanol and DCM with a gradient of 0-10%. The isolated product was triturated with ethyl acetate and the solid was collected by filtration and dried in vacuo to give 7-[2-((Z)-3-diethylaminoprop-1-enyl)-4-fluorobenzenesulfonylamino]-4H-furo[2,3-c]chromene-6-carboxylic acid (0.056 g) as a white solid.

1. customthe mixture was irradiated in the microwave at 130° C. for 1 hour
2. temperatureAfter cooling
3. customevaporated to dryness
4. customThe residue was triturated with 10% methanol in DCM
5. filtrationfiltered
6. customthe filtrate was evaporated to dryness
7. customThe residue was purified by chromatography on silica
8. washeluting with a mixture of methanol and DCM with a gradient of 0-10%
9. customThe isolated product was triturated with ethyl acetate
10. filtrationthe solid was collected by filtration
11. customdried in vacuo