HRID53593

反应详情

EQUATION

反应方程式

HRID 53593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solution was evaporated
  2. additionthe residue was treated with 40% NaOH to pH=12
  3. filtrationThe mixture was filtered
  4. customthe solid was dried
  5. customto leave a yellow solid
  6. filtrationthe mixture was filtered
  7. customThe filtrate was evaporated