反应详情

温度

40 °C

A mixture of this ethylenediamine (31 g, 0.137 mole) and triethylamine (28 g, 0.277 mole) was added dropwise over 30 minutes to a stirred solution of ethyl-2,3-dibromopropionate (35.0 g, 0.135 mole) dissolved in 200 mL of toluene and heated to 40° C. After the addition was complete, the reaction was heated at 80°-85° C. for 7 hours, cooled to room temperature, and partitioned between water and toluene. The organic layer was separated, dried, and stripped of all solvent under reduced pressure to yield 38 g of the crude product. Chromatographic purification gave 12.8 g of ethyl 1-phenyl-4-(phenylmethyl)-2-piperazinecarboxylate.

1. additionAfter the addition
2. temperaturethe reaction was heated at 80°-85° C. for 7 hours
3. temperaturecooled to room temperature
4. custompartitioned between water and toluene
5. customThe organic layer was separated
6. customdried
7. customto yield 38 g of the crude product
8. customChromatographic purification