HRID1908813

反应详情

EQUATION

反应方程式

HRID 1908813 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2,5-dichloro-4-hydroxypyridine (1.43 g, 8.73 mmol) in DMF (15 mL), K2CO3 (2.41 g, 17.5 mmol) followed by methyl iodide (1.48 g, 8.73 mmol) is added. The mixture is stirred at rt for 24 h before it is diluted with EA (200 mL), washed with water (2×100 mL), dried over MgSO4, filtered and concentrated. The crude product is purified by CC on silica gel eluting with heptane:EA 1:1 to give 2,5-dichloro-4-methoxy-pyridine (0.73 g) as a white solid; LC-MS: tR=0.85 min; [M+1]+=177.90.

WORKUP

后处理

  1. additionis added
  2. washwashed with water (2×100 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude product is purified by CC on silica gel eluting with heptane:EA 1:1