反应详情

温度

80 °C

A mixture of methyl 7-[2-(3-diethylaminopropyl)-4-fluorobenzenesulfonylamino]-furo[2,3-c]quinoline-6-carboxylate (Intermediate 71, 0.100 g) and lithium hydroxide monohydrate (0.250 g) in dioxane (4 mL) and water (1.25 mL) was heated at 80° C. overnight. The mixture was cooled and saturated aqueous ammonium chloride was added. This was concentrated in vacuo and the residue was triturated with DCM and methanol, filtered and the filtrate was concentrated in vacuo. The residue was purified by HPLC (C6 Ph) eluting with a mixture of methanol and water containing 0.1% formic acid, with a gradient of 10-40% to give a yellow gum. The product was triturated with ether to give 7-[2-(3-diethylaminopropyl)-4-fluorobenzenesulfonyl-amino]-furo[2,3-c]quinoline-6-carboxylic acid (0.045 g) as a yellow solid.

1. temperatureThe mixture was cooled
2. concentrationThis was concentrated in vacuo
3. customthe residue was triturated with DCM and methanol
4. filtrationfiltered
5. concentrationthe filtrate was concentrated in vacuo
6. customThe residue was purified by HPLC (C6 Ph)
7. washeluting with a mixture of methanol and water containing 0.1% formic acid, with a gradient of 10-40%
8. customto give a yellow gum
9. customThe product was triturated with ether