HRID1156346

反应详情

EQUATION

反应方程式

HRID 1156346 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5.5 parts of 3-(2-chloroethyl)-2-phenyl-4(3H)-quinazolinone, 3.2 parts of 3-(4-piperidinyl)-1H-indole, 7 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 22 hours. The reaction mixture is filtered over Hyflo and the filtrate is evaporated. The residue is purified by column-chromatography over silic gel using a mixture of trichloromethane and methanol (92:8 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from a mixture of ethanol and 1,1'-oxybisethane, yielding 5 parts of 3-[2-[4-(1H-indol-3-yl)-1-piperidinyl]ethyl]-2-phenyl-4(3H)-quinazolinone; mp. 191.3° C.

WORKUP

后处理

  1. temperaturerefluxed for 22 hours
  2. filtrationThe reaction mixture is filtered over Hyflo
  3. customthe filtrate is evaporated
  4. customThe residue is purified by column-chromatography over silic gel
  5. additiona mixture of trichloromethane and methanol (92:8 by volume) as eluent
  6. customThe pure fractions are collected
  7. customthe eluent is evaporated
  8. customThe residue is crystallized from a mixture of ethanol and 1,1'-oxybisethane