反应详情

Hydrogen chloride (4M in dioxane, 2 ml) was added to a solution of 6-(benzenesulphonylmethyl)-2-[2-(t-butoxycarbonyl)aminoethoxy]-3-(furan-3-yl)benzoic acid (Intermediate 6, 0.018 g) in dioxane (0.5 ml) and the resultant mixture was stirred at room temperature for 2 hours. The mixture was evaporated to dryness and the residue was triturated with ether. The solid was collected by filtration then purified by chromatography on silica, eluting with a mixture of DCM, methanol, acetic acid and water in a ratio of 240:20:3:2 changing to 120:15:3:2. After evaporation of the solvent, the residue was treated with hydrochloric acid (1M) and evaporated to dryness to give 2-(2-aminoethoxy)-6-(benzenesulphonylmethyl)-3-(furan-3-yl)benzoic acid hydrochloride (0.008 g) as a white solid.

1. customThe mixture was evaporated to dryness
2. customthe residue was triturated with ether
3. filtrationThe solid was collected by filtration
4. customthen purified by chromatography on silica
5. washeluting with a mixture of DCM, methanol, acetic acid and water in a ratio of 240:20:3:2 changing to 120:15:3:2
6. customAfter evaporation of the solvent
7. additionthe residue was treated with hydrochloric acid (1M)
8. customevaporated to dryness