HRID413474

反应详情

EQUATION

反应方程式

HRID 413474 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride (0.65 g, 0.0167 moles) was added slowly to a well-stirred solution of 2-chloro-5-methylpyridine-3-carbaldehyde (1.3 g, 0.0084 moles) in methanol (20 ml) at 0° C. temperature over a period of 15 minutes. The reaction mass was further stirred for 2 hours at the same temperature. The solvent was removed under reduced pressure and the mass was quenched with water (25 ml). The mass was extracted with ethyl acetate (2×50 ml) and the layers separated. The organic layer was removed under reduced pressure. The residue so obtained was subjected to chromatographic purification on silica gel to give 2-chloro-3-hydroxymethyl-5-methylpyridine as a solid in 88 % yield.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customthe mass was quenched with water (25 ml)
  3. extractionThe mass was extracted with ethyl acetate (2×50 ml)
  4. customthe layers separated
  5. customThe organic layer was removed under reduced pressure
  6. customThe residue so obtained
  7. customwas subjected to chromatographic purification on silica gel