HRID611586

反应详情

EQUATION

反应方程式

HRID 611586 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5,6-Dichloro-2-(1-t-butyloxycarbonyl-2-(R)-pyrrolidinyl)furo[3,2-b]pyridine (355 mg, 1.0 mmol) was dissolved in CH2Cl2 (3 mL) and TFA (3 mL) was added at ambient temperature. After stirring for 1 hour, the solvent was removed and the residue was redissolved in CH2Cl2 and washed with saturated K2CO3 solution, dried (MgSO4) and concentrated. The crude product was chromatographed (silica gel; CHCl3 /MeOH, 98:2) to afford a solid (220 mg, 87%): 1H NMR (CDCl3, 300 MHz) δ 1.81-2.05 (m, 3H), 2.15-2.29 (m, 1H), 3.04-3.20 (m, 2H), 4.39-4.42 (m, 1H), 6.70 (s, 1H), 7.80 (s, 1H); MS (CI/NH3) m/z: 257 (M+H)+.

WORKUP

后处理

  1. customthe solvent was removed
  2. dissolutionthe residue was redissolved in CH2Cl2
  3. washwashed with saturated K2CO3 solution
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customThe crude product was chromatographed (silica gel; CHCl3 /MeOH, 98:2)