反应详情

To a solution of 2-chloro-5-hydroxy-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide (WO 99/29661) (0.30 g), triphenylphosphine (0.25 g) and 2-chloroethanol (0.07 ml) in tetrahydrofuran (4 ml) was added diethyl azodicarboxylate (0.15 ml) and the reaction mixture stirred at room temperature for 18 h. Further triphenylphosphine (0.12 g) and diethyl azodicarboxylate (0.08 ml) were added and the reaction stirred for an additional 4 h. Silica was added and the reaction mixture concentrated under reduced pressure. The residue was purified by silica gel chromatography (eluting with 20% ethyl acetate in isohexanes) to deliver the sub-title compound as a lightly coloured oil (0.31 g).

1. stirringthe reaction stirred for an additional 4 h
2. additionSilica was added
3. concentrationthe reaction mixture concentrated under reduced pressure
4. customThe residue was purified by silica gel chromatography (eluting with 20% ethyl acetate in isohexanes)