反应详情

温度

60 °C

A solution of 2-azidomethyl-3-phenylbenzo[b]thiophene (244 mg, 0.92 mmol) in THF (10 mL) was treated with a solution of triphenylphosphine (302 mg, 1.15 mmol) in water (1 mL) under a nitrogen atmosphere. The mixture was heated at 60° C. for 2 h then cooled to RT. The volatiles were removed in vacuo and the resulting residue loaded onto an Isolute® SCX-2 cartridge then washed with MeOH and the product eluted with 2M NH3/MeOH. The product containing fractions were combined and concentrated in vacuo affording the title compound (288 mg, quantitative). LCMS (Method C): RT 2.15 min [M−N3]+ 223.0.

1. temperaturethen cooled to RT
2. customThe volatiles were removed in vacuo
3. washthen washed with MeOH
4. washthe product eluted with 2M NH3/MeOH
5. additionThe product containing fractions
6. concentrationconcentrated in vacuo