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
10.0 g (34 mmol) of methyl 2-(2-chlorobenzyloxy)-5-fluorobenzoate are dissolved in 80 ml of methanol and 40 ml of 40% strength sodium hydroxide solution and stirred at RT for 12 h. The solvent is distilled out in vacuo, water is added to the residue until it has all dissolved, and the solution is then extracted with ethyl acetate. The aqueous phase is acidified with hydrochloric acid and extracted three times with ethyl acetate. The mixture is dried over magnesium sulfate, filtered, washed with ethyl acetate and concentrated. The residue is mixed with petroleum ether, and the crystals which have separated out are filtered off with suction and dried on a clay dish. 6.00 g (21.3 mmol, 63% of theory) of the title compound are obtained.
WORKUP
后处理
- distillationThe solvent is distilled out in vacuo, water
- additionis added to the residue until it
- extractionthe solution is then extracted with ethyl acetate
- extractionextracted three times with ethyl acetate
- dry with materialThe mixture is dried over magnesium sulfate
- filtrationfiltered
- washwashed with ethyl acetate
- concentrationconcentrated
- additionThe residue is mixed with petroleum ether
- customthe crystals which have separated out
- filtrationare filtered off with suction
- customdried on a clay dish