HRID1966237
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
5-Chloro-2-nitro-pyridine-3-ol (5.7 mmol) is dissolved in THF (35 ml) and triphenylphosphin (2 eq.) and 1-Methoxy-2-propanol (1 eq.) is added at 0° C. After addition of di-tert.-butylazodicarboxylate (1.5 eq) in THF (10 ml), the reaction is stirred five hours at 0° C. The solvent is removed in vacuo. 5-Chloro-3-(2-methoxy-1-methyl-ethoxy)-2-nitro-pyridine is obtained after column chromatography (heptan/ethylacetate) as yellow solid in a yield of 100%. HPLC (method C): 1.81 min; LC-MS (method A): 1.64 min, 247.05 (MH+).
WORKUP
后处理
- customThe solvent is removed in vacuo