HRID402394

反应详情

EQUATION

反应方程式

HRID 402394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of [5-(5-fluoro-pyridin-2-yl)-3-methyl-3H-[1,2,3]triazol-4-yl]-methanol (416 mg, 2.0 mmol), 5-hydroxy-pyridine-2-carboxylic acid ethyl ester (362 mg, 2.60 mmol) and triphenylphosphine (682 mg, 2.6 mmol) in THF (10 mL) was added diethyl azodicarboxylate (40% in toluene, 1.19 mL, 2.6 mmol) dropwise at 0° C. The reaction mixture was then stirred at room temperature for 1 h and then evaporated. Purification by chromatography (silica, 50 to 100% ethyl acetate in heptane) afforded the title compound (386 mg, 77%) as a white solid after recrystallisation from ethyl acetate. MS: m/e=358.3 [M+H]+.

WORKUP

后处理

  1. customevaporated
  2. customPurification by chromatography (silica, 50 to 100% ethyl acetate in heptane)