反应详情

Hydrazine (64.1 g, 2 mol) was added dropwise, over 8–10 min, to methyl 3-morpholinopropionate (35 g, 0.202 mol) and the reaction mixture was refluxed for 16 h. The excess hydrazine was removed under reduced pressure and the material was dried in vacuo at room temperature for 16 h to give the crude product as an oil. The 1H NMR showed the presence of hydrazine, so the crude material was dried using a lyophilizer. Then the oil was refluxed in benzene/water (using a Dean-Stark distilling receiver). The benzene was then removed under reduced pressure, and the product was triturated with petroleum ether. After sitting in petroleum ether at room temperature for 16 h, the oil solidified. The petroleum ether was decanted and the solid was dried under house vacuum at room temperature to give the desired product (21.5 g, 61.4%), which was used without further purification.

1. temperaturethe reaction mixture was refluxed for 16 h
2. customThe excess hydrazine was removed under reduced pressure
3. customthe material was dried in vacuo at room temperature for 16 h
4. customto give the crude product as an oil
5. dry with materialso the crude material was dried
6. temperatureThen the oil was refluxed in benzene/water (
7. distillationdistilling receiver)
8. customThe benzene was then removed under reduced pressure
9. customthe product was triturated with petroleum ether
10. customThe petroleum ether was decanted
11. customthe solid was dried under house vacuum at room temperature