HRID40750
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
- 130 °C
PROCEDURE
实验过程
A mixture of 3-bromo-5-fluorobenzonitrile (1.6 g, 7.8 mmol), piperidine-4-carboxylic acid (2.6 g, 12.0 mmol), triethylamine (4.0 mL, 28.5 mmol) and N,N-dimethylacetamide (1.5 mL) in a sealed tube was heated to 130° C. for 48 hr. The reaction mixture was diluted with EtOAc and water. The organic layer was separated, dried (MgSO4), and concentrated to give a crude reside which was purified by chromatography on silica gel (CH2Cl2/MeOH) to afford 1-(3-bromo-5-cyanophenyl)piperidine-4-carboxylic acid.
WORKUP
后处理
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customto give a crude reside which
- customwas purified by chromatography on silica gel (CH2Cl2/MeOH)