HRID2356633

反应详情

EQUATION

反应方程式

HRID 2356633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium carbonate (82 mg) was added to a solution of (6-cyano-5-methyl-2-pyridinyl)methyl acetate (3.62 g) in methanol (25 ml) and the mixture stirred under argon at ambient temperature for 2 hours. It was concentrated in vacuo to ca. ¼ volume and water (50 ml) added. The mixture was neutralized with 5% acetic acid (1.5 ml) and extracted with dichloromethane (50 ml then 2×25 ml). The combined extracts were washed with brine (25 ml), dried (MgSO4) and concentrated in vacuo. The residue was recrystallised from ether:hexane to afford the title compound (2.26 g, 80%) as a pale buff solid.

WORKUP

后处理

  1. concentrationIt was concentrated in vacuo to ca. ¼ volume and water (50 ml)
  2. additionadded
  3. extractionextracted with dichloromethane (50 ml
  4. washThe combined extracts were washed with brine (25 ml)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was recrystallised from ether