HRID16086
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 1-bromo-4-fluoro-3-(trifluoromethyl)benzene (5.02 g) and potassium cyanide (1.38 g) in DMSO (20 ml) was heated at 80° C. for 14 h. Water was added and the mixture was extracted ether, the organic extracts were dried (MgSO4) and evaporated to give a brown oil. This was dissolved in DMSO (10 ml) and 4 M NaOH (10 ml) and heated at 100° C. for 16 h. 2 M Hcl (20 ml) was added and the mixture was extracted with DCM (three times), the organic extracts were dried (MgSO4), evaporated and purified by chromatography (silica, CH2Cl2-MeOH—AcOH as eluent) to give the sub-title compound (1.99 g).
WORKUP
后处理
- extractionthe mixture was extracted ether
- dry with materialthe organic extracts were dried (MgSO4)
- customevaporated
- customto give a brown oil
- addition2 M Hcl (20 ml) was added
- extractionthe mixture was extracted with DCM (three times)
- dry with materialthe organic extracts were dried (MgSO4)
- customevaporated
- custompurified by chromatography (silica, CH2Cl2-MeOH—AcOH as eluent)