反应详情

温度

50 °C

A mixture of 3,3-dimethyl-1-(9-oxa-3,7-diazabicyclo[3.3.1]non-3-yl)-2-butanone (from step (ii) above; 56 mg, 0.25 mmol), TEA (0.35 mL, 2.5 mmol) and MeCN (2 mL) was treated with 4-cyanophenethyl methanesulfonate (see step (iii) above; 84 mg, 0.37 mmol). The resulting mixture was stirred at 50° C. for 24 h. The solvents were removed by evaporation, the crude product was dissolved in DCM and then the solution was added to an ion-exchange solid-phase extraction plug (2 g, CBA (carboxylic acid on silica support)). After 1 h, the plug was washed with DCM (15 mL), after which the product was finally eluted with DCM:MeOH:TEA (90:5:5), to give 84 mg (95%) of the title compound.

1. customThe solvents were removed by evaporation
2. dissolutionthe crude product was dissolved in DCM
3. additionthe solution was added to an ion-exchange solid-phase extraction plug (2 g, CBA (carboxylic acid on silica support))
4. waitAfter 1 h
5. washthe plug was washed with DCM (15 mL)
6. washafter which the product was finally eluted with DCM:MeOH:TEA (90:5:5)