反应详情

A 100 mL round bottom flask containing 2-[(2,3-Dihydro-benzofuran-7-ylmethyl)-amino]-indan-2-carboxylic acid ethyl ester (367, 350 mg, 1.037 mmol) is charged with 1,4-dioxane (3 mL) and MeOH (3 mL). A stirring bar is added and stirring is initiated. After dissolution, water (1.5 mL) is added followed by the LiOH monohydrate (110 mg, 2.52 mmol). After 16 h, tlc analysis (silica, 50% EtOAc/Heptanes) indicates that the starting material is completely consumed. Amberlyst highly acidic exchange resin (0.5 g) is added to the reaction vial. The reaction is capped and allowed to stir at ambient temperature. After 6 h, the contents of the flask are filtered through a pad of Celite. The solvent is removed from the filtrate. The residue is reconstituted with iPrOH/toluene (20+20 mL) and the solvent is removed. This process is repeated 1 time. Pumping to constant weight provided white solid (0.31 g, 99%).

1. additionA stirring bar is added
2. additionis added
3. customis completely consumed
4. additionAmberlyst highly acidic exchange resin (0.5 g) is added to the reaction vial
5. customThe reaction is capped
6. stirringto stir at ambient temperature
7. waitAfter 6 h
8. filtrationthe contents of the flask are filtered through a pad of Celite
9. customThe solvent is removed from the filtrate
10. customthe solvent is removed