反应详情

To a mixture of triphenylphosphine (0.79 g, 3.0 mmol) in THF (15 ml) was successively added diisopropylazodicarboxylate (0.61 g, 3.0 mmol) followed by methyl salicylate (0.46 g, 3.0 mmol) and the resultant mixture stirred at ambient temperature for 1 h. 1-(2-Hydroxyethyl)-pyrrolidine (0.35 g, 3.0 mmol) was then added drop-wise and the reaction mixture left stirring at ambient temperature for a further 5 h. The reaction mixture was reduced in vacuo and purified by flash column chromatography [SiO2, EtOAc/MeOH (3:1, 1:1)] to give 2-(2-pyrrolidin-1-yl-ethoxy)-benzoic acid methyl ester as a clear yellow oil (446 mg, 60%). (LC/MS: Rt 1.58, [M+H]+ 250.05).

1. waitthe reaction mixture left
2. custompurified by flash column chromatography [SiO2, EtOAc/MeOH (3:1, 1:1)]