HRID558115
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
Mix 2-(2-bromo-4-fluoro-phenyl)-2-methyl-propionitrile (1 g, 4.13 mmol) and 1,4,7,10,13,16-hexaoxacyclooctadecane (18-crown-6) (100 mg, 1% wt) with sodium hydroxide (10 M, 20 mL, 200 mmol) in ethanol (5 mL). Heat the mixture to reflux for 3 h. Quench the reaction with 1 N HCl. Extract the product with chloroform. Dry the organic phase over sodium sulfate and concentrate to give an oily residue. Purify the residue by FCC (10% methanol in DCM as eluant) to give the title compound as a yellow solid (1 g, 93%). MS (ES) m/z 260/262 [M+1]+.
WORKUP
后处理
- temperatureHeat the mixture
- temperatureto reflux for 3 h
- customQuench
- customthe reaction with 1 N HCl
- extractionExtract the product with chloroform
- dry with materialDry the organic phase over sodium sulfate
- concentrationconcentrate
- customto give an oily residue
- customPurify the residue by FCC (10% methanol in DCM as eluant)