HRID611586
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
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
- customthe solvent was removed
- dissolutionthe residue was redissolved in CH2Cl2
- washwashed with saturated K2CO3 solution
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe crude product was chromatographed (silica gel; CHCl3 /MeOH, 98:2)