HRID53593
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
- 70 °C
PROCEDURE
实验过程
A mixture of 1.16 g (6.04 mmol) of 2-amino-4,6-dimethyl-3-nitro-5-pyridinecarbonitrile (17) and 5.72 g (30.1 mmol) of SnCl2 in 15 mL of ethanol was heated at 70° C. for 1 h. The solution was evaporated and the residue was treated with 40% NaOH to pH=12. The mixture was filtered and the solid was dried to leave a yellow solid. The solid was stirred with ethyl acetate (100 mL) and the mixture was filtered. The filtrate was evaporated to leave a pale yellow solid (410 mg, 41%). 1H NMR (CDCl3), 2,334 (s, 3), 2.522 (s, 3), 3.151 (mb, 2), 4.65 (mb, 2).
WORKUP
后处理
- customThe solution was evaporated
- additionthe residue was treated with 40% NaOH to pH=12
- filtrationThe mixture was filtered
- customthe solid was dried
- customto leave a yellow solid
- filtrationthe mixture was filtered
- customThe filtrate was evaporated