反应详情

A 100 mL Parr reaction vessel is charged with 2-(Isoquinolin-5-ylcarbamoyl)-indan-2-carboxylic acid ethyl ester (320, 500 mg, 1.39 mmol) and EtOH (10 mL). The reaction vessel is agitated by swirling until dissolution ° C. curred. Acetic acid (10 mL) and platinum (IV) oxide (117 mg, 0.52 mmol) are added. The vessel is fitted on a Parr hydrogenation apparatus, flushed with N2 and then evacuated. The vessel is charged with hydrogen to 50 psi. The apparatus is set to agitate. After 4 h, agitation is ceased. The reaction vessel is evacuated and flushed with nitrogen. This process is repeated. The contents of the reaction vessel are diluted with iPrOH (50 mL) and filtered through a pad of celite. Solvent is removed from the filtrate under reduced pressure. The resulting residue is reconstituted in iPrOH (15 mL) and toluene (15 mL). The solvent is removed under reduced pressure. This process is repeated. Pumping to constant weight yields light beige solid (0.5 g, 99%).

1. customA 100 mL Parr reaction vessel
2. dissolutionby swirling until dissolution ° C
3. customThe vessel is fitted on a Parr hydrogenation apparatus
4. customflushed with N2
5. customevacuated
6. additionThe vessel is charged with hydrogen to 50 psi
7. stirringto agitate
8. customThe reaction vessel is evacuated
9. customflushed with nitrogen
10. additionThe contents of the reaction vessel are diluted with iPrOH (50 mL)
11. filtrationfiltered through a pad of celite
12. customSolvent is removed from the filtrate under reduced pressure
13. customThe solvent is removed under reduced pressure