反应详情

A solution of toluene-4-sulfonic acid (1R,2R)-2-benzyloxycarbonylamino-cyclohexylmethyl ester (632 mg, 1.51 mmol) in acetone (8 mL) was treated with N-[3-(4-fluorophenyl)-propyl]-methylamine (253 mg, 1.51 mmol) and potassium carbonate (209 mg, 1.51 mmol) and heated at reflux for 23.5 hours. The mixture was cooled and filtered, the solid was rinsed with acetone, and the filtrate was concentrated to provide a yellow-orange oil. Flash chromatography on silica gel, eluting with 50% ethyl acetate in hexane, followed by 50% ethyl acetate in hexane containing 5% ethanol, provided a light yellow viscous oil (400 mg, 64%).

1. temperatureheated
2. temperatureat reflux for 23.5 hours
3. temperatureThe mixture was cooled
4. filtrationfiltered
5. washthe solid was rinsed with acetone
6. concentrationthe filtrate was concentrated
7. customto provide a yellow-orange oil
8. washFlash chromatography on silica gel, eluting with 50% ethyl acetate in hexane