HRID2204686
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of methyl 2-(acetyloxy)-4-bromo-5-(bromomethyl)benzoate (may be prepared as described in Description 16; 741 mg, 2.03 mmol) in acetone (5 ml) was added triethylamine (0.56 ml, 4.05 mmol) and morpholine (0.23 ml, 2.63 mmol). The mixture was stirred for 1 hour, then the solvent was removed in vacuo to give a residue. The residue was redissolved in ethyl acetate (10 ml) and washed with water (10 ml). The organic layer was dried (MgSO4) and the solvent removed in vacuo to give oil. Purification by column chromatography (SiO2, 3:1-1:1 cyclohexane/ethyl acetate) gave the product as oil. 580 mg.
WORKUP
后处理
- customthe solvent was removed in vacuo
- customto give a residue
- washwashed with water (10 ml)
- dry with materialThe organic layer was dried (MgSO4)
- customthe solvent removed in vacuo
- customto give oil
- customPurification by column chromatography (SiO2, 3:1-1:1 cyclohexane/ethyl acetate)