HRID384674

反应详情

EQUATION

反应方程式

HRID 384674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trimethylacetyl chloride (4.22 g, 35.0 mmol) was added dropwise to a solution of 2-amino-4-chloropyridine (3.00 g, 23.3 mmol) in pyridine (11 mL) at 0° C. The resulting solution was stirred for 12 h at r.t. Water (20 mL) was added and the aqueous phase was extracted with ethyl acetate (3×10 mL). The combined organic extracts were dried (MgSO4). The solvent was removed in vacuo and the crude mixture was purified by flash chromatography on silica, eluting with ethyl acetate and hexane (2/8), to give the title compound as a colourless solid (4.9 g, 99%).

WORKUP

后处理

  1. extractionthe aqueous phase was extracted with ethyl acetate (3×10 mL)
  2. dry with materialThe combined organic extracts were dried (MgSO4)
  3. customThe solvent was removed in vacuo
  4. customthe crude mixture was purified by flash chromatography on silica
  5. washeluting with ethyl acetate and hexane (2/8)