HRID350338
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 stirred solution of 1-(tert-butoxycarbonyl)-2-[2-(4-ethoxycarbonylphenyl) ethynyl]pyrrolidine (2.75 g, 8 mmol) in CH2Cl2 (5 mL) was added TFA (5 mL), and the resulting mixture was stirred overnight. The mixture was concentrated in vacuo and made basic with sat. NaHCO3 and extracted with CHCl3. The extract was washed with brine, dried over MgSO4, evaporated to give 1.95 g (q.y.) 2-[2-(4-ethoxycarbonylphenyl) ethynyl]pyrrolidine as a light yellow oil. 1H-NMR (CDCl3) δ 1.38 (3 H, t, J=6.8 Hz), 1.82–2.16 (4 H, m), 3.01–3.48 (2 H, m), 4.00–4.11 (1 H, m), 4.37 (2H, q, J=6.8 Hz), 4.54–4.77 (1 H, m), 7.44–7.46 (2 H, m), 7.95–7.97 (2 H, m).
WORKUP
后处理
- concentrationThe mixture was concentrated in vacuo
- extractionextracted with CHCl3
- washThe extract was washed with brine
- dry with materialdried over MgSO4
- customevaporated