HRID1886193

反应详情

EQUATION

反应方程式

HRID 1886193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl potassium malonate (57 mg) was suspended in dry tetrahydrofuran (1 ml) and 2M isopropyl magnesium chloride in THF (170 μl) added. The suspension was sonicated for 1/2 hour giving a homogenous solution. This was added with stirring to the suspension of 6-(2-methylimidazo[4,5-c]pyrid-1-yl)pyrid-3-oyl chloride in dichloromethane. The mixture was stirred at room temperature for 1/2 hour. It was then poured into 1N hydrochloric acid, stirred for 15 minutes and adjusted to pH 8 with saturated sodium bicarbonate. The aqueous phase was extracted with dichloromethane (2×10 ml), the extracts combined, dried over magnesium sulphate and the solvent removed under reduced pressure yielding the title compound as a pale red oil (40 mg, 63%) [as a 1:1 mixture of enol and keto tautomers].

WORKUP

后处理

  1. customThe suspension was sonicated for 1/2 hour
  2. customgiving a homogenous solution
  3. additionThis was added
  4. stirringstirred for 15 minutes
  5. extractionThe aqueous phase was extracted with dichloromethane (2×10 ml)
  6. dry with materialdried over magnesium sulphate
  7. customthe solvent removed under reduced pressure