HRID422100
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
- 60 °C
PROCEDURE
实验过程
Treat a solution of 2-chloro-4-iodo-5-methoxymethoxy-pyridine (8.1 g, 27 mmol) in THF (40 mL) with 3 N HCl (61 mL). Heat the resulting mixture to 60° C. for 3 hours. Cool the mixture to room temperature and adjust the pH to 7 by the slow addition of saturated aqueous sodium bicarbonate solution. Extract the mixture with three portions of ethyl acetate. Combine the organic extracts and dry over sodium sulfate, filter, and concentrate in vacuo to give the title compound (6.8 g, 98%) as a brown solid used without further purification. 1H NMR (400 MHz, DMSO-d6) δ 11.04 (s, 1H), 7.81-7.87 (m, 2H).
WORKUP
后处理
- temperatureCool the mixture to room temperature
- extractionExtract the mixture with three portions of ethyl acetate
- dry with materialdry over sodium sulfate
- filtrationfilter
- concentrationconcentrate in vacuo