HRID712750
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
5-Bromo-4-chloro-pyridine-3-carbaldehyde (500 mg, 2.27 mmol) is dissolved in MeOH (20 mL) and sodium borohydride (257 mg, 6.80 mmol) is added. The mixture is stirred for 1 hr at room temperature and the solvent is removed in vacuo. Then saturated NH4Cl aqueous solution (20 mL), water (50 mL) and EtOAc (50 mL) are added and the mixture is stirred for 10 min. The aqueous layer is separated and extracted with EtOAc (2×50 mL). The organic layers are combined and concentrated to give the crude product. Purification by flash column chromatography affords 400 mg of (5-bromo-4-chloro-pyridin-3-yl)-methanol.
WORKUP
后处理
- customthe solvent is removed in vacuo
- additionThen saturated NH4Cl aqueous solution (20 mL), water (50 mL) and EtOAc (50 mL) are added
- stirringthe mixture is stirred for 10 min
- customThe aqueous layer is separated
- extractionextracted with EtOAc (2×50 mL)
- concentrationconcentrated
- customto give the crude product
- customPurification by flash column chromatography