反应详情

A solution of n-butyllithium in toluene (20%; 65.6 g; 0.20 mol) is added over the course of from 10 to 15 min to a solution of 31 g of N-benzylpiperidine (0.175 mol) in 60 ml of tert-butyl methyl ether. The reaction mixture is heated at from 55° to 60° C. for approximately 18 h and then metered at RT into a cold (-20° C.) solution of 50.1 g of diethyl oxalate (0.42 mol) in 160 ml of toluene. The mixture is heated to RT and stirred at from 20° to 25° C. for 30 min. Acetic acid (100%; 12.6 g; 0.21 mol) and a mixture of 50 g of crushed ice and 100 g of water are then added to the reaction mixture. The phases are separated and the organic phase is washed with 50 ml of water and concentrated by evaporation in vacuo: 43.2 g (content 89%; yield 80%).

1. temperatureThe reaction mixture is heated at from 55° to 60° C. for approximately 18 h
2. additionare then added to the reaction mixture
3. customThe phases are separated
4. washthe organic phase is washed with 50 ml of water
5. concentrationconcentrated by evaporation in vacuo