HRID473402

反应详情

EQUATION

反应方程式

HRID 473402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Methyl-3-nitropyridine (24 g, 173.91 mmol) was dissolved in 1,4-dioxane (500 mL) and to the mixture was added selenium dioxide (23 g, 208.7 mmol) and the mixture was heated under reflux for 16 h. After completion of reaction, the mixture was cooled to rt and filtered through Celite™ and the filtrate was concentrated under reduced pressure to give thick oily mass. The oily mass was purified by silical gel column chromatography using 20% of ethyl acetate and hexane as eluent to give 3-nitro-2-pyridinecarbaldehyde as an off white solid: 1H-NMR (CDCl3) δ: 7.7 (m, 1H), 8.3 (d, 1H), 9.0 (d, 1H), 10.3 (s, 1H).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 16 h
  3. customAfter completion of reaction
  4. filtrationfiltered through Celite™
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customto give thick oily mass
  7. customThe oily mass was purified by silical gel column chromatography