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 to 60° C. for 2 h and then cooled to RT. Volatile were removed under reduced pressure and the resulting residue was loaded onto an Isolute® SCX-2 cartridge which was washed with MeOH and the product eluted with 2M NH3/MeOH. The product containing fractions were combined and concentrated in vacuo affording (3-phenylbenzo[b]thiophen-2-yl)methanamine (288 mg, quantitative). LCMS: RT 2.15 min [M-N3]+ 223.0

1. temperaturecooled to RT
2. customVolatile were removed under reduced pressure
3. washwas washed with MeOH
4. washthe product eluted with 2M NH3/MeOH
5. additionThe product containing fractions
6. concentrationconcentrated in vacuo