HRID1966254
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
- 105 °C
PROCEDURE
实验过程
5-(4-Methanesulfonyl-phenoxy)-3-(2-methoxy-ethoxy)-2-nitro-pyridine (0.39 mmol) is dissolved in acetic acid (4 ml). After addition of water (1.2 ml), zinc powder (6.3 eq.) is added and the reaction suspension is heated to 105° C. for 90 minutes. The reaction suspension is cooled to room temperature and filtrated. The filtrate is pored into 3.5% NaOH (30 ml) and extracted with dichloromethane. The combined organic layers are washed with brine, dried over MgSO4 and the solvent is removed in vacuo. 5-(4-Methanesulfonyl-phenoxy)-3-(2-methoxy-ethoxy)-pyridine-2-ylamine is obtained as yellow oil in a yield of 96%. HPLC (method C): 1.21 min, LC-MS (method A): 0.55 min, 339.15 (MO.
WORKUP
后处理
- additionis added
- temperatureThe reaction suspension is cooled to room temperature
- filtrationfiltrated
- extractionextracted with dichloromethane
- washThe combined organic layers are washed with brine
- dry with materialdried over MgSO4
- customthe solvent is removed in vacuo