反应详情

A 100 mL round bottom flask which contains 2-[(3-propoxy-pyridine-2-carbonyl)-amino]-indan-2-carboxylic acid ethyl ester (332, 620 mg, 1.68 mmol) is charged with 1,4-dioxane (6 mL) and MeOH (6 mL). A stirring bar is added and stirring is initiated. After dissolution, water (3 mL) is added followed by the LiOH monohydrate (178 mg, 4.25 mmol). After 22 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 flask. The reaction is capped and allowed to stir at ambient temperature. After 125 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+10 mL) and the solvent is removed. This process is repeated 1 time. Pumping to constant weight provides 0.58 g of white solid.

1. customA 100 mL round bottom flask which contains
2. additionA stirring bar is added
3. additionis added
4. customis completely consumed
5. additionAmberlyst highly acidic exchange resin (0.5 g) is added to the reaction flask
6. customThe reaction is capped
7. stirringto stir at ambient temperature
8. waitAfter 125 h
9. filtrationthe contents of the flask are filtered through a pad of Celite
10. customThe solvent is removed from the filtrate
11. customthe solvent is removed