HRID1732746

反应详情

EQUATION

反应方程式

HRID 1732746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 5-methoxy-4-oxo-10-propyl-6,7,8,9-tetrahydro-4H-naphtho[2,3-b]pyran-2-carboxylic acid (5 g) in 48% aqueous hydrobromic acid (130 ml) was heated under reflux for 7 hours. The reaction mixture was cooled and excess saturated aqueous sodium bicarbonate added. The resulting solution was filtered, the filtrate acidified with concentrated hydrochloric acid and then extracted with chloroform (100 ml). The chloroform solution was dried (Na2SO4) and evaporated leaving a residue which, when crystallised from acetone, gave the title compound as an orange crystalline solid mp 259°-260°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 7 hours
  3. temperatureThe reaction mixture was cooled
  4. filtrationThe resulting solution was filtered
  5. extractionextracted with chloroform (100 ml)
  6. dry with materialThe chloroform solution was dried (Na2SO4)
  7. customevaporated
  8. customleaving a residue which, when
  9. customcrystallised from acetone