反应详情

A mixture of N-[(2S)-5-hydroxy-2,3-dihydro-1H-inden-2-yl]-2-propanesulfonamide (120 mg, 0.470 mmol, Description 3) and 3-pyridinylmethanol (51.3 mg, 0.470 mmol) in dichloromethane (10 ml) was stirred under argon at room temperature. Triphenylphosphine (123 mg, 0.470 mmol) and diisopropyl azodicarboxylate (0.091 ml, 0.470 mmol) were then successively added. The resulting mixture was stirred at room temperature under argon for 16 hours. The reaction mixture was washed with water, dried over sodium sulphate, filtered and evaporated. The desired product was purified by column chromatography on silica eluting with 1 to 99% ethyl acetate in n-pentane and then by SCX column eluting with 1M ammonia in methanol solution to give the title compound as a white solid. The free base solid was dissolved in methanol and treated with ethereal hydrochloride to give the HCl salt (64 mg).

1. stirringThe resulting mixture was stirred at room temperature under argon for 16 hours
2. washThe reaction mixture was washed with water
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customevaporated
6. customThe desired product was purified by column chromatography on silica eluting with 1 to 99% ethyl acetate in n-pentane
7. washby SCX column eluting with 1M ammonia in methanol solution