反应详情

温度

60 °C

2-Methyl-1,2-propanediamine (0.12 ml) was added to a solution of 2-chloro-5-[3-[(methylsulfonyl)oxy]propyl]-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide (0.250 g, Example 6e) in tetrahydrofuran (4 ml) and heated at 60° C. in a sealed tube for 12 h. On cooling to ambient temperature, the mixture was diluted with ethyl acetate and extracted twice with saturated sodium hydrogencarbonate solution and once with brine, dried over magnesium sulfate and concentrated under reduced pressure. Purification by preparative reverse phase HPLC (eluting with a gradient of acetonitrile in 0.1% aqueous ammonium acetate/25–95%) gave the title compound as the acetate salt. Treatment with 4M hydrochloric acid in dioxane gave the title compound as the dihydrochloride salt (0.045 g).

1. temperatureOn cooling to ambient temperature
2. extractionextracted twice with saturated sodium hydrogencarbonate solution and once with brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customPurification by preparative reverse phase HPLC (
6. washeluting with a gradient of acetonitrile in 0.1% aqueous ammonium acetate/25–95%)