HRID466186
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
The ketone (2.53 g, 9.5 mmol) is dissolved in 90 ml of an EtOH/pyridine mixture (1:1), and treated with hydroxylamine hydrochloride (0.99 g, 14.3 mmol). The mixture is stirred for 2 days. The reaction mixture is partitioned between ether and water, and the aqueous layer is extracted twice with ether. The combined organic layer is then washed twice with 2N HCl and water, dried (MgSO4), and evaporated. The residue is purified by flash chromatography (10% EtOAc/hexane) to give 3-acetyl-6-phenoxy-2H-1-benzopyran oxime as a crystalline solid.
WORKUP
后处理
- customThe reaction mixture is partitioned between ether and water
- extractionthe aqueous layer is extracted twice with ether
- washThe combined organic layer is then washed twice with 2N HCl and water
- dry with materialdried (MgSO4)
- customevaporated
- customThe residue is purified by flash chromatography (10% EtOAc/hexane)