反应详情

温度

100 °C

3-(2-Methoxy-1-methyl-ethoxy)-2-nitro-5-phenoxy-pyridine (0.4 mmol) is dissolved in acetic acid (1.5 ml). After addition of water (1.5 ml), zinc powder (6 eq.) is added and the reaction suspension is heated to 100° 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 extracted with brine, dried over MgSO4 and the solvent is removed in vacuo. 3-(2-Methoxy-1-methyl-ethoxy)-5-phenoxy-pyridine-2-ylamine is obtained as yellow powder in a yield of 64%. HPLC (method C): 1.51 min, LC-MS (method A): 0.923 min, 275.15 (MH+).

1. additionis added
2. temperatureThe reaction suspension is cooled to room temperature
3. filtrationfiltrated
4. extractionextracted with dichloromethane
5. extractionThe combined organic layers are extracted with brine
6. dry with materialdried over MgSO4
7. customthe solvent is removed in vacuo