HRID1253155
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis refluxed for three hours
- additionthe pH added to 8-10
- extractionextracted with methylene chloride
- extractionThe organic extract
- washis washed with sat'd NaCl
- customdried
- filtrationfiltered
- customevaporated
- customthe residue chromatographed (silica gel, hexane/ether)