反应详情

温度

-60 °C

A solution of 1 g. (0.003 mole) of trans-2-(3,4-dimethoxybenzyl)-5-[2-(4-methoxyphenyl)ethyl]pyrrolidine hydrochloride in 35 ml. of methylene chloride was cooled to -65° C. and treated with 2.68 g. (0.012 mole) of boron tribromide dropwise. The reaction mixture was then stirred under N2 and slowly warmed from -65° to room temperature over the course of one hour and 25 minutes. The solution was then cooled again to -60° C. and 25 ml. of methanol was cautiously added. Solvent was removed in vacuo, more methanol was added and some insoluble material was filtered off. After removal of methanol in vacuo, the residue was treated with ethyl acetate. Upon standing at room temperature, 0.8 g. of product was obtained as an off-white solid, m.p. 202°-203° C.

1. additiontreated with 2.68 g
2. temperatureslowly warmed from -65° to room temperature over the course of one hour and 25 minutes
3. customSolvent was removed in vacuo, more methanol
4. additionwas added
5. filtrationsome insoluble material was filtered off
6. customAfter removal of methanol in vacuo
7. additionthe residue was treated with ethyl acetate
8. customUpon standing at room temperature
9. customof product was obtained as an off-white solid, m.p. 202°-203° C.