HRID1992678
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
Lithium hydroxide (171 mg, 7.14 mmol) was added to a solution of methyl (3S,4R)-4-(2,4-difluorophenyl)-1-isopropylpyrrolidine-3-carboxylate, from preparation 32 (1.01 g, 3.59 mmol) in tetrahydrofuran (10 mL) at room temperature. The reaction mixture was stirred for 3 hours and the solvent was removed in vacuo. The residue was dissolved in water (20 mL) and washed with ethyl acetate (2×20 mL). The phases were separated and the aqueous phase was acidified with 2M aqueous hydrochloric acid solution (3.59 mL) and extracted with ethyl acetate (20 mL). The organic extracts were combined, dried over magnesium sulfate and concentrated in vacuo to afford the desired product as a foam, 686 mg (71%).
WORKUP
后处理
- customthe solvent was removed in vacuo
- dissolutionThe residue was dissolved in water (20 mL)
- washwashed with ethyl acetate (2×20 mL)
- customThe phases were separated
- extractionextracted with ethyl acetate (20 mL)
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo