Triphenylphosphine → HCID 90997563, compound

Participants

Reaction Steps

By a procedure similar to that for 9a, compound 8b (1.67 g, 4.8 mmol) was treated with Ph3P (2.42 g, 9.2 mmol), freshly distilled DIAD (1.86 g, 9.2 mmol) and DPPA (2.54 g, 9.2 mmol) in THF (45 mL) for 48 h at room temperature to give the corresponding azide product (1.39 g, 78% yield) after purification by flash column chromatography (60% EtOAc/hexane, 3:2). The subsequent hydrolysis in refluxing EtOH/HCl (1 M aqueous solution) gave the desired product 9b (1.18 g, 95% yield), which was used directly for the preparation of 10b.

Provenance & Evidence