HRID1659208

反应详情

EQUATION

反应方程式

HRID 1659208 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1.92 g of 5-aminosalicylic acid and 5.0 g of tautomeric 1-[3,4-dihydro-1-(2-oxo-2-phenylethyl)-2(1H)-naphthalenylidene]pyrrolidinium bromide in equilibrium with 1-phenacyl-2-(1-pyrrolidino)-3,4-dihydronaphthalene hydrobromide (Example 1a), in 75 ml of methanol is refluxed under nitrogen for 9 hours. The solution is allowed to reach ambient temperature before being filtered. The methanol is removed under a vacuum to give a viscous oil which is dissolved in acetonitrile. This solution immediately crystallizes to give a yellow crystalline solid which is collected by filtration and washed with acetonitrile to give 3-(3-carboxy-4-hydroxyphenyl)-4,5-dihydro-2-phenylbenz[e]indole.

WORKUP

后处理

  1. customto reach ambient temperature
  2. filtrationbefore being filtered
  3. customThe methanol is removed under a vacuum
  4. customto give a viscous oil which
  5. customThis solution immediately crystallizes
  6. customto give a yellow crystalline solid which
  7. filtrationis collected by filtration
  8. washwashed with acetonitrile