HRID632505
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
To 100 mL of ethanol were added 10.0 g of 1-methylpiperazine and 20.2 g of triethylamine. To the mixture cooled with ice, 25 mL of a solution of 24.6 g of 4-(bromomethyl)-2-methoxy-benzoic acid methyl ester in ethanol was added dropwise. The mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated. To the residue, 75 mL of water and 250 mL of methylene chloride were added, and the organic layer was separated. The obtained organic layer was dried over Na2SO4 and concentrated. The residue was purified by amino-silica gel column chromatography (heptane/AcOEt system) to give 22.4 g of the title compound (85% yield).
WORKUP
后处理
- additionwas added dropwise
- concentrationThe reaction mixture was concentrated
- additionTo the residue, 75 mL of water and 250 mL of methylene chloride were added
- customthe organic layer was separated
- dry with materialThe obtained organic layer was dried over Na2SO4
- concentrationconcentrated
- customThe residue was purified by amino-silica gel column chromatography (heptane/AcOEt system)