反应详情

温度

90 °C

Lithium hydroxide monohydrate (0.107 g) was added to a solution of methyl 7-[2-((Z)-3-diethylaminoprop-1-enyl)-4-fluorobenzenesulfonylamino]-furo[2,3-c]-quinoline-6-carboxylate (Intermediate 6, 0.026 g) in a mixture of dioxane (1.7 mL) and water (0.8 mL). The resultant mixture was stirred and heated at 90° C. overnight. After cooling, the mixture was acidified by addition of formic acid and then evaporated to dryness. The residue was triturated with a mixture of methanol and DCM (10%) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of methanol and DCM with a gradient of 0-12%. The product was triturated with a mixture of DCM and diethyl ether (50%) and the solid was collected by filtration and dried in vacuo to give 7-[2-((Z)-3-diethylaminoprop-1-enyl)-4-fluorobenzenesulfonylamino]-furo[2,3-c]quinoline-6-carboxylic acid (0.013 g) as a yellow solid.

1. temperatureAfter cooling
2. customevaporated to dryness
3. customThe residue was triturated with a mixture of methanol and DCM (10%)
4. filtrationfiltered
5. customThe filtrate was evaporated to dryness
6. customthe residue was purified by chromatography on silica
7. washeluting with a mixture of methanol and DCM with a gradient of 0-12%
8. customThe product was triturated with a mixture of DCM and diethyl ether (50%)
9. filtrationthe solid was collected by filtration
10. customdried in vacuo