HRID361970
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 2,6-dichlorobenzoylchloride (5.24 g; 25 mmol), 3-methylanisole(2.44 g; 20 mmol) and iron(III)chloride (20 mg) is heated to 100° C.for 45 minutes with stirring. After cooling, toluene is added, the mixture is shaken with water, the organic phase is dried and the solvent is evaporated. The reaction product is purified chromatograpically (flash column with 70 g of silicagel; elution with petrolether/toluene changing from 75:25 to 40:60 (v/v)). After evaporation the residue from the main fraction is treated with petrolether to give white crystals (1.33 g; 22.5%y); mp. 89° C.
WORKUP
后处理
- temperatureAfter cooling
- customthe organic phase is dried
- customthe solvent is evaporated
- customThe reaction product is purified chromatograpically
- wash(flash column with 70 g of silicagel; elution with petrolether/toluene changing from 75:25 to 40:60 (v/v))
- customAfter evaporation the residue from the main fraction
- additionis treated with petrolether
- customto give white crystals (1.33 g; 22.5%y)