HRID418998

反应详情

EQUATION

反应方程式

HRID 418998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A magnetically stirred mixture of (2,4-dimethyl-pyridin-3-yl)-methanol (0.342 g, 2.5 mmol) and IBX (1.40 g, 5 mmol) in acetonitrile (5 mL) placed in a round bottom flask was heated at 80° C. in an oil bath for 1 h. The mixture was cooled to room temperature and filtered. The solid was washed with acetonitrile. The filtrate was concentrated and applied to a short silica gel column and chromatographed using hexane/ethyl acetate solvent mixture (30-60% ethyl acetate). Product containing fractions were combined and the solvent was evaporated to afford 0.283 g of 2,4-dimethyl-pyridine-3-carbaldehyde as a white solid. MS: (M+H)/z=136.

WORKUP

后处理

  1. customplaced in a round bottom flask
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationfiltered
  4. washThe solid was washed with acetonitrile
  5. concentrationThe filtrate was concentrated
  6. customchromatographed
  7. additionProduct containing fractions
  8. customthe solvent was evaporated