HRID1255836
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
A mixture of methyl 3-{1-[(6-chloropyrazin-2-yl)amino]ethyl}benzoate (30 mg, 0.1 mmol) in dilute aqueous sodium hydroxide (0.5 mL, 2M, 1 mmol), methanol (2 mL) and dichloromethane (1 mL) was stirred at room temperature for 16 hours. After this time the mixture was concentrated under reduced pressure and the residue was dissolved in water (5 mL) which was then acidified to pH 6 with dilute aqueous hydrochloric acid (1M). The aqueous solution was extracted with ethyl acetate (3×10 mL) and the extracts were washed with brine (10 mL), dried (MgSO4) and concentrated under reduced pressure to give 3-{1-[(6-chloropyrazin-2-yl)amino]ethyl}benzoic acid (11 mg, 41%) as a beige coloured oil.
WORKUP
后处理
- concentrationAfter this time the mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in water (5 mL) which
- extractionThe aqueous solution was extracted with ethyl acetate (3×10 mL)
- washthe extracts were washed with brine (10 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure