HRID1459724

反应详情

EQUATION

反应方程式

HRID 1459724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvents were removed in vacuo
  2. dissolutionthe residue was dissolved in dichloromethane (25 ml)
  3. washwashed with 2N NaOH solution (10 ml)
  4. washthe combined organic extracts were washed with saturated NaCl solution (10 ml)
  5. dry with materialdried (Na2SO4)
  6. customevaporated in vacuo