HRID1820871

反应详情

EQUATION

反应方程式

HRID 1820871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.16 g (0.36 mmol) of 3-biphenyl-4-ylpropynoic acid-[3-chloro-4-(2-diethylaminoethoxy)phenyl]amide (educt XII.1) is dissolved in 10 mL of aqueous ethanol and 0.10 mL (1.0 mmol) of piperidine is added. The mixture is stirred for 8 hours at reflux temperature. After cooling, the solvent is eliminated, and the residue is suspended in ether and filtered off. The residue is dried in vacuo at 50° C. Yield: 75 mg (45% of theory); Rf value: 0.40 (silica gel, methylene chloride/methanol/ammonia=9:1:0.01); m.p. 148° C.-151° C.; C27H29ClN2O3; EII mass spectrum: m/z=465/467 [M+H]+.

WORKUP

后处理

  1. temperatureat reflux temperature
  2. temperatureAfter cooling
  3. filtrationfiltered off
  4. customThe residue is dried in vacuo at 50° C