HRID858830

反应详情

EQUATION

反应方程式

HRID 858830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Prepared according to a procedure reported for related compounds: Henichart, J. P. et al. J. Het Chem. 1977, 14, 615. Methyl isothiocyanate (9.08 g, 0.124 mol) in EtOH (50 mL) was added at room temperature to a stirred solution of 3-morpholin-4-ylpropanohydrazide (21.5 g, 0.124 mol) in EtOH (200 mL). The mixture was refluxed for 8 h, then removed from heat and stirred at room temperature for 16 h. The EtOh was removed under reduced pressure to give the crude material as a yellow oil. The oil was purified by column chromatography through silica gel, eluting with CH2Cl2/MeOH to afford the title compound. (6 g, 21.2%).

WORKUP

后处理

  1. customPrepared
  2. temperatureThe mixture was refluxed for 8 h
  3. customremoved
  4. temperaturefrom heat
  5. customThe EtOh was removed under reduced pressure
  6. customto give the crude material as a yellow oil
  7. customThe oil was purified by column chromatography through silica gel
  8. washeluting with CH2Cl2/MeOH