HRID7839

反应详情

EQUATION

反应方程式

HRID 7839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A suspension of 9a-butyl-7-methoxy-4-(4-methoxymethoxy-phenyl)-1,2,9,9a-tetrahydro-3H-fluoren-3-one (813 mg, 2 mmol) in methanol (12 mL) was warmed in an oil bath at 60° C. and treated with aqueous 2N HCl (4 mL). The resulting mixture was stirred and heated at 60° C. for two hours, then cooled to room temperature and evaporated under vacuum to leave a yellow semi-solid. The residue was dissolved in EtOAc, washed with water and brine, dried over MgSO4, filtered, evaporated under vacuum, and stripped with toluene to afford 9a-butyl-4-(4-hydroxy-phenyl)-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (787 mg, ca. 92% weight pure) as a yellow foam.

WORKUP

后处理

  1. temperatureheated at 60° C. for two hours
  2. temperaturecooled to room temperature
  3. customevaporated under vacuum
  4. customto leave a yellow semi-solid
  5. washwashed with water and brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated under vacuum