反应详情

温度

60 °C

A solution of 0.20 g (0.88 mmol) of 3-[(1-naphthalenyloxy)methyl]pyrrolidine, prepared in Step 12.2., and 0.35 g (1.5 mmol) of ethyl [(phenyloxycarbonyl)oxy]acetate, prepared in accordance with Example 1.1, in 6 ml of toluene is heated at 60° C. overnight. It is evaporated to dryness and the residue is taken up in a mixture of water, dichloromethane and saturated aqueous sodium hydrogen carbonate solution. The organic phase is decanted, dried over sodium sulfate and evaporated to dryness. The residue is purified by chromatography on a silica gel column, eluting with dichloromethane and then with a 99/1 mixture of dichloromethane and methanol. This gives 0.24 g of product in oil form, which is used as it is in the following step.

1. customIt is evaporated to dryness
2. additionthe residue is taken up in a mixture of water, dichloromethane and saturated aqueous sodium hydrogen carbonate solution
3. customThe organic phase is decanted
4. dry with materialdried over sodium sulfate
5. customevaporated to dryness
6. customThe residue is purified by chromatography on a silica gel column
7. washeluting with dichloromethane
8. additionwith a 99/1 mixture of dichloromethane and methanol