反应详情

A mixture of 2-fluoro-4-[4-methyl-5-(2-{3-methyl-4-[(4-methyl-2,6,7-trioxabicyclo[2.2.2]oct-1-yl)methoxy]phenyl}ethyl)thien-2-yl]benzonitrile (intermediate 101, 0.016 g) in 2-propanol (2 ml) was treated with 2M aqueous hydrochloric acid (1 ml) and the mixture stirred at reflux for 2 hours. The solvent was removed and the residue dissolved in 1,4-dioxane (2 ml) and water (1 ml). This mixture was treated with 2M aqueous sodium hydroxide (0.5 ml) and the mixture stirred for 16 hours). The solvent was removed and the residue purified by SPE (aminopropyl). The title compound, as the free acid, was recovered by treating a solution of this product with Dowex H+.

1. temperatureat reflux for 2 hours
2. customThe solvent was removed
3. dissolutionthe residue dissolved in 1,4-dioxane (2 ml)
4. additionThis mixture was treated with 2M aqueous sodium hydroxide (0.5 ml)
5. stirringthe mixture stirred for 16 hours)
6. customThe solvent was removed
7. customthe residue purified by SPE (aminopropyl)
8. customThe title compound, as the free acid, was recovered
9. additionby treating a solution of this product with Dowex H+