反应详情

Diethyl azodicarboxylate (41.0 ml) was added to a solution of triphenylphosphine (62.9 g) in tetrahydrofuran (800 ml) at 0° C. After 15 minutes 3,4-dichlorophenol (39.1 g) was added, after a further 15 minutes tert-butyl 4-hydroxy-1-piperidinecarboxylate (48.3 g) in tetrahydrofuran (400 ml) was added dropwise over 30 min. The solution was stirred at room temperature for 16 hours and concentrated to a small volume. Purification by chromatography (ethyl acetate:iso-hexane 95:5) gave the sub-title compound as an oil (61.3 g).

1. additionwas added dropwise over 30 min
2. concentrationconcentrated to a small volume
3. customPurification by chromatography (ethyl acetate:iso-hexane 95:5)