HRID709047

反应详情

EQUATION

反应方程式

HRID 709047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,3-Dimethoxy-5-[(trimethylsilyl)ethynyl]pyridine (Intermediate 31) (9.8 g, 42 mmol) was dissolved in a mixture of aqueous sodium hydroxide (21 ml, 2 M, 42 mmol) and methanol (50 ml) to give a colourless solution which was stirred for 16 hours. The reaction was evaporated and the residue was partitioned between ethyl acetate and water before the organic layer was dried and concentrated in vacuo. The crude material was purified by (SiO2; 0-10% ethyl acetate in petrol) to afford 5-ethynyl-2,3-dimethoxypyridine (5.6 g, 82%).

WORKUP

后处理

  1. customto give a colourless solution which
  2. customThe reaction was evaporated
  3. customthe residue was partitioned between ethyl acetate and water before the organic layer
  4. customwas dried
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by (SiO2; 0-10% ethyl acetate in petrol)