HRID583180
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
2-Bromo-3-methoxy-6-nitropyridine (470 mg, 2.0 mmol) was added to 8 mL (3:1 water: ethanol) and 2 mL of 30% ammonium hydroxide. Added 350 mg (2 mmol) of sodium hydrosulfite (Na2SsO4) and heated to 60° C. After 30 min, no starting material was seen. Added 50 mL of water and extracted the product with methylene chloride (2×25 mL). Dried over MgSO4, filtered and reduced the volume. Flash chromatography (75/25 hexane/ethyl acetate) recovered 200 mg of product (50% yield). 1H NMR (CDCl3, 200 MHz) δ 7.06 (d, 1H, 10 Hz), 6.41 (d, 1H, J=10 Hz), 3.8 (s, 3H) ppm
WORKUP
后处理
- extractionextracted the product with methylene chloride (2×25 mL)
- dry with materialDried over MgSO4
- filtrationfiltered