HRID54513

反应详情

EQUATION

反应方程式

HRID 54513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.8 g of 2-[2'-(1H-imidazol-1-yl)acetyl]-5-chloropyridine in 40 ml of methanol is charged at 0°, in portions, with 2.0 g of sodium borohydride. The mixture is stirred for one hour at 0°. For working-up the mixture is decomposed by careful addition of 1N hydrochloric acid at 0°, followed by 1N sodium hydroxide to reach a pH of 9. The solvents are evaporated in vacuo. The residue is stirred with water and dichloromethane, the aqueous phase is extracted twice with dichloromethane and the combined organic extracts are washed with brine, dried and evaporated. The compound is obtained as a cream coloured solid; m.p.: >210° (decomp.). Purification is possible by chromatography over silicagel.

WORKUP

后处理

  1. customThe solvents are evaporated in vacuo
  2. stirringThe residue is stirred with water and dichloromethane
  3. extractionthe aqueous phase is extracted twice with dichloromethane
  4. washthe combined organic extracts are washed with brine
  5. customdried
  6. customevaporated
  7. customThe compound is obtained as a cream
  8. customPurification