反应详情

温度

100 °C

2-Hydroxy-2-methyl-1-propylamine [prepared according to Journal American Chemical Society (1941), 63, p1034] (0.25 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 6 e) in butan-1-ol (8 ml) and heated at 100° C. in a sealed tube for 24 h. On cooling to ambient temperature, the mixture was diluted with ethyl acetate and extracted twice with saturated aqueous sodium hydrogencarbonate solution and once with brine, dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by solid phase extraction on SCX resin and preparative reverse phase HPLC (eluting with a gradient of acetonitrile in 0.1% aqueous ammonium acetate/25-95%) to give the title compound as the acetate salt (0.160 g).

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