反应详情

A mixture of 5-(azidomethyl)-3-(5-chloropyridin-2-yl)-1,3-oxazolidin-2-one (139 mg, INTERMEDIATE 2) and triphenylphosphine (226 mg) was heated to 65° C. for 8 h in 66 ml of tetrahydrofuran and 9 ml of water. The sample was then cooled to room temperature, and concentrated in vacuo. The residue was purified via column chromatography on a Biotage Horizon 40M column eluting with 100% ethyl acetate (5 column volumes) to remove excess triphenylphosphine and triphenylphosphine oxide, followed by 100% methanol (5 column volumes), to provide the title compound (122 mg, 94%). Mass spectrum (ESI) 228.0 (M+1).

1. concentrationconcentrated in vacuo
2. customThe residue was purified via column chromatography on a Biotage Horizon 40M column
3. washeluting with 100% ethyl acetate (5 column volumes)
4. customto remove excess triphenylphosphine and triphenylphosphine oxide