HRID1455008
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
To a solution of the subtitle product of step ii) (2.0 g) in DCM (20 ml) and sodium bicarbonate (1.36 g) in water (20 ml) at 0° C. was added dimethylamine (1.00 ml, 40% aqueous) dropwise. The reaction mixture was stirred at room temperature for 2 h before DCM (40 ml) was added and the aqueous layer separated. The organic layer was washed with water (20 ml), brine (10 ml) and dried (MgSO4). The solid was filtered and the solvent evaporated to dryness under reduced pressure. The residue was purified by column chromatography (EtOAc/isohexane (1:1)) to yield the subtitle compound as an off white solid. Yield 1.9 g
WORKUP
后处理
- additionwas added
- customthe aqueous layer separated
- washThe organic layer was washed with water (20 ml), brine (10 ml)
- dry with materialdried (MgSO4)
- filtrationThe solid was filtered
- customthe solvent evaporated to dryness under reduced pressure
- customThe residue was purified by column chromatography (EtOAc/isohexane (1:1))