HRID477981

反应详情

EQUATION

反应方程式

HRID 477981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.36 g of 5-(p-hydroxymethylphenyl)imidazo[1,5-a]pyridine in 25 ml of ethanol and 6.4 ml of concentrated hydrochloric acid is hydrogenated with 0.15 g 10% palladium on charcoal at 40 psi of hydrogen and 60° for 4 h. The reaction mixture is filtered and evaporated and the residue is partitioned between methylene chloride and sodium bicarbonate solution. The organic phase is dried over sodium sulfate and evaporated to an oil which is purified by preparative layer chromatography on silica with ethyl acetate. The hydrochloride salt is prepared in acetone with 1.1 molar equivalents of ethereal hydrogen chloride to yield the title compound, m.p. 173°-175°.

WORKUP

后处理

  1. filtrationThe reaction mixture is filtered
  2. customevaporated
  3. customthe residue is partitioned between methylene chloride and sodium bicarbonate solution
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customevaporated to an oil which
  6. customis purified by preparative layer chromatography on silica with ethyl acetate