HRID5847

反应详情

EQUATION

反应方程式

HRID 5847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,4,5-trimethoxyphenylisocyanate (420 mg; 2.0 mmol) (produced as in Example 1) and 3-[4-(2-chloro-phenyl) -1-piperazinyl]propanol (500 mg; 20 mmol) in toluene (25 ml) was refluxed for 16 h. The solvent was evaporated and the residue taken up in ethanol, which was treated with hydrogen chloride in ether. Recrystallization from ethanol/ether afforded 400 mg of the title compound. M.p. 185°-187° C. MS (70 eV): m/z 463 (6%, M+), 254 (30), 209 (100), 194 (52), 166 (34), 70 (58).

WORKUP

后处理

  1. temperaturewas refluxed for 16 h
  2. customThe solvent was evaporated
  3. additionwhich was treated with hydrogen chloride in ether
  4. customRecrystallization from ethanol/ether