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 solution of (3R)-1-(tert-butoxycarbonyl)-3-[(4-fluorobenzylthio)methyl]pyrrolidine (0.5422 g, 1.67 mmol) in 90% formic acid (5 ml) was stirred at room temperature for 23 h. The solvents were removed in vacuo and the residue was dissolved in dichloromethane (25 ml) and washed with 2N NaOH solution (10 ml). The aqueous layer was reextracted with more dichloromethane (25 ml) and the combined organic extracts were washed with saturated NaCl solution (10 ml), dried (Na2SO4) and evaporated in vacuo to leave 0.3903 g of the title compound as an oil. δH (360 MHz, CDCl3) 1.42 (1H, m), 1.94 (1H, m), 2.24 (1H, m), 2.45 (2H, m), 2.59 (1H, m), 2.92 (2H, m), 3.08 (1H, m), 3.69 (2H, s), 7.00 (2H, t, J=8.6 Hz), 7.25-7.29 (2H, m).
WORKUP
后处理
- customThe solvents were removed in vacuo
- dissolutionthe residue was dissolved in dichloromethane (25 ml)
- washwashed with 2N NaOH solution (10 ml)
- washthe combined organic extracts were washed with saturated NaCl solution (10 ml)
- dry with materialdried (Na2SO4)
- customevaporated in vacuo