反应详情

Sodium azide (179 mg, 2.76 mmol) was added to a solution of methanesulfonic acid 3-phenylbenzo[b]thiophen-2-ylmethyl ester (828 mg, 1.84 mmol) in DMF (10 mL) and the mixture stirred at RT for 18 h. The reaction mixture was diluted with water and extracted with EtOAc. The organic fraction was washed with brine, dried (Na2SO4) and concentrated in vacuo and the resulting residue purified by column chromatography (Si—PCC, gradient 0-35% DCM in cyclohexane) affording the title compound as a clear oil (244 mg, 50%). LCMS (Method C): RT 4.46 min [M+H-N2]+ 237.8

1. extractionextracted with EtOAc
2. washThe organic fraction was washed with brine
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customthe resulting residue purified by column chromatography (Si—PCC, gradient 0-35% DCM in cyclohexane)