HRID72457
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 an ice cooled solution of methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate (D72) (165 mg, 0.520 mmol) in methanol (10 ml), 10N NaOH (10 ml) was added. The mixture was heated under reflux overnight. After cooled to room temperature, the mixture was concentrated in vacuo. The residue was diluted with water (10 ml), acidified with 2.5N HCl (pH 1-2), and the resulting mixture was extracted with ethyl acetate (2×10 ml). The organic solution was washed with brine (20 ml), dried over Na2SO4 and evaporated in vacuo to afford the title compound (D98) (170 mg) as a red solid.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux overnight
- concentrationthe mixture was concentrated in vacuo
- additionThe residue was diluted with water (10 ml)
- extractionthe resulting mixture was extracted with ethyl acetate (2×10 ml)
- washThe organic solution was washed with brine (20 ml)
- dry with materialdried over Na2SO4
- customevaporated in vacuo