HRID1920879
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
PROCEDURE
实验过程
2,2,2-trifluoro-1-(2-fluoro-4-iodo-3-pyridyl)ethanol (45 g, 140.2 mmol) was dissolved in anhydrous toluene (1 L). Manganese (IV) oxide (143.4 g, 1.402 mol) was added portionwise with rapid stirring. The mixture was heated to reflux for 3 hours and then allowed to cool and filtered through a plug of celite. The solid residues were washed with EtOAc and the filtrate was concentrated to a deep red oil which was slurried in petrol and then filtered to give a white solid impurity. The filtrate was concentrated to give the product as a red oil (40 g, 89% Yield).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 3 hours
- temperatureto cool
- filtrationfiltered through a plug of celite
- washThe solid residues were washed with EtOAc
- concentrationthe filtrate was concentrated to a deep red oil which
- filtrationfiltered
- customto give a white solid impurity
- concentrationThe filtrate was concentrated