HRID2204338
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 (5-bromo-6-methoxy-pyridin-3-yl)-acetic acid (Step AN2) (400 mg, 1.6 mmol) in CH2Cl2 (0.8 mL) was added DCC (18 mg, 0.09 mmol), DMAP (one spatula) and EtOH (4.88 mmol) and the mixture was stirred at rt for 15 h. H2O and EtOAc were added and the phases were separated. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated. The residue was purified by flash chromatography (heptane/EtOAc, 85:15→0:100). ESI-MS: tR=1.05 min, [M+H]+ 274.1/276.1 (LC-MS 1).
WORKUP
后处理
- customthe phases were separated
- washThe organic layer was washed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by flash chromatography (heptane/EtOAc, 85:15→0:100)