HRID1980056
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
Into a 300 ml four-necked flask, there were charged benzene (200 ml), 4-fluoro-α,α-dimethylbenzylamine (7.7 g) and triethylamine (6.0 g), and o-methylphenylacetyl chloride (9.5 g) was dropwise added thereto at room temperature while stirring, followed by refluxing for 3 hours. After cooling, the reaction mixture was washed with water to remove triethylamine hydrochloride. After the benzene layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was recrystallized from ethanol to give 11.3 g of N-(4-fluoro-α,α-dimethylbenzyl)-o-methylphenylacetamide (Compound No. 11). M.P., 150°-151° C.
WORKUP
后处理
- additionwas dropwise added
- temperatureby refluxing for 3 hours
- temperatureAfter cooling
- washthe reaction mixture was washed with water
- customto remove triethylamine hydrochloride
- dry with materialAfter the benzene layer was dried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was recrystallized from ethanol