HRID1501037
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 the solution of 4-(1-hydroxyethyl)benzoate (300 mg. 1.67 mmol) in tetrahydrofuran (50 mL) was added triphenylphosphine (570 mg, 2.2 mmol) and o-cresol (180 mg, 1.67 mmol), the mixture was stirred for 30 minutes at room temperature, then diisopropylazodicarboxylate (568.3 mg, 2.2 mmol) was added dropwise to the solution at 0° C., the mixture was stirred at room temperature for 12 hours. Then the mixture was concentrated and purified by column chromatography (silica gel, Petroleum ether/ethyl acetate=20:1) to give methyl 4-(1-(o-tolyloxy)ethyl)benzoate (151 mg, 33%) as oil.
WORKUP
后处理
- stirringthe mixture was stirred at room temperature for 12 hours
- concentrationThen the mixture was concentrated
- custompurified by column chromatography (silica gel, Petroleum ether/ethyl acetate=20:1)