反应详情

温度

60 °C

A mixture of 3-benzyl-3,8-diazabicyclo[3.2.1]octane (3.46 g, 17.1 mmol; from Preparation B, step (e) above) and 4-(2-oxiranylmethoxy)benzonitrile (3.00 g, 17.1 mmol; prepared as described in international patent application WO 99/31100) in 2-propanol (70 mL) and H2O (7 mL) was stirred at 60° C. for 22 h. The reaction mixture was concentrated in vacuo. The residue was dissolved in CH2Cl2 (200 mL) and washed with water (50 mL) and brine (50 mL). The organic layer was dried (NaSO4), filtered and concentrated in vacuo to give the crude product. Flash chromatography on silica gel eluting with CH2Cl2:CMA (8:1) gave 5.74 g (89%) of the sub-title compound as a yellow oil.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionThe residue was dissolved in CH2Cl2 (200 mL)
3. washwashed with water (50 mL) and brine (50 mL)
4. dry with materialThe organic layer was dried (NaSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customto give the crude product