HRID1898599
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
- 120 °C
PROCEDURE
实验过程
To a solution of 2-bromopyridin-4-ol (1.6 g, 9.2 mmol) and (bromomethyl)cyclopropane (1.61 g, 12.0 mmol) in DMF (12 mL) in a microwave vial was added cesium carbonate (4.19 g, 12.9 mmol). The vial was sealed and heated in a microwave reactor at 120° C. for 4 h. The reaction mixture was cooled to room temperature, quenched with water and extracted with EtOAc (2×). The combined organics were washed with sat'd NaCl then dried over MgSO4 and concentrated. The residue was purified by SiO2 chromatography (20-50% EtOAc/heptane) to give 1.45 g (69%) of 2-bromo-4-cyclopropylmethoxy-pyridine as a yellow oil.
WORKUP
后处理
- customThe vial was sealed
- temperatureThe reaction mixture was cooled to room temperature
- customquenched with water
- extractionextracted with EtOAc (2×)
- washThe combined organics were washed with sat'd NaCl
- dry with materialthen dried over MgSO4
- concentrationconcentrated
- customThe residue was purified by SiO2 chromatography (20-50% EtOAc/heptane)