HRID1253155

反应详情

EQUATION

反应方程式

HRID 1253155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the 4-methoxy compound from Step 3 above (5 g) and 48% aq. HBr (50 ml) in glacial acetic acid (50 ml) is refluxed for three hours. The mixture is poured into H2O, the pH added to 8-10 and extracted with methylene chloride. The organic extract is washed with sat'd NaCl, dried, filtered, evaporated and the residue chromatographed (silica gel, hexane/ether) affording the desired product as a green solid.

WORKUP

后处理

  1. temperatureis refluxed for three hours
  2. additionthe pH added to 8-10
  3. extractionextracted with methylene chloride
  4. extractionThe organic extract
  5. washis washed with sat'd NaCl
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customthe residue chromatographed (silica gel, hexane/ether)