HRID65677

反应详情

EQUATION

反应方程式

HRID 65677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred solution of tetrahydro-3,5-bis[(4-methoxy-2,5-dimethylphenyl)methylene]-4H-pyran-4-one (3.0 g, 7.6 mmole) and 2-amino-2-thiazoline (1.0 g, 9.7 mmole) in 75 ml of CHCl3 is heated at reflux temperature for 72 hours. After cooling, the solution is filtered to remove a small amount of insoluble material. The solvent is evaporated to give an oily residue. A solution of this material in 25 ml of EtOH yields 1.7 g of light yellow solid, m.p. 195°-197°. Crystallization from 20 ml of 10% DMF/MeOH gives 1.3 g (35%) of cream colored solid, m.p. 196°-198°.

WORKUP

后处理

  1. temperatureat reflux temperature for 72 hours
  2. temperatureAfter cooling
  3. filtrationthe solution is filtered
  4. customto remove a small amount of insoluble material
  5. customThe solvent is evaporated
  6. customto give an oily residue