反应详情

温度

65 °C

Borane tetrahydrofuran complex 1M (0.714 ml, 0.714 mmol) was added to a stirred solution of 1-[2-(4-nitrophenyl)ethyl]-4-[2-(4-nitrophenyl)propanoyl]piperazine (92 mg, 0.22 mmol) in THF then refluxed for 1 hr. LC-MS and TLC showed starting material left. More borane-THF complex 1M (0.71 ml, 0.71 mmol) was added to the reaction and refluxed for 5 hrs. The reaction was cooled and added 6N HCl and then warmed to 65° C. for 0.5 hour. The reaction was poured into 1N NaOH and extracted with ethyl acetate. The ethyl acetate layer was washed with water and brine then dried and concentrated. The residue was purified by mass directed HPLC. LC-MS (IE, m/z): 399 [M+1]+. (0.34 μM)

1. temperaturethen refluxed for 1 hr
2. waitleft
3. additionMore borane-THF complex 1M (0.71 ml, 0.71 mmol) was added to the reaction
4. temperaturerefluxed for 5 hrs
5. temperatureThe reaction was cooled
6. extractionextracted with ethyl acetate
7. washThe ethyl acetate layer was washed with water and brine
8. customthen dried
9. concentrationconcentrated
10. customThe residue was purified by mass