反应详情

3-Aminopropanol (1ml) was added to a solution of 2-chloro-5-[3-[(methylsulfonyl)oxy]propyl]-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide (0.270 g, Example 6e) in tetrahydrofuran (30 ml) and the solution heated to reflux for 12 h. On cooling to ambient temperature the reaction mixture was diluted with water and extracted thrice with dichloromethane. The organic extracts were combined, dried over magnesium sulfate and concentrated under reduced pressure. Purification by preperative reverse phase HPLC eluting with a gradient of acetonitrile/0.1% aqueous ammonium acetate (25-95%), gave the title compound as the acetate salt. Treatment with 4 M hydrochloric acid in dioxane gave the title compound as the hydrochloride salt (0.070 g).

1. temperaturethe solution heated
2. temperatureto reflux for 12 h
3. extractionextracted thrice with dichloromethane
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customPurification by preperative reverse phase HPLC
7. washeluting with a gradient of acetonitrile/0.1% aqueous ammonium acetate (25-95%)