反应详情

A solution of [(S)-3-benzyloxy-1-(4-fluoro-2-phenylaminophenylcarbamoyl)propyl]carbamic acid tert-butyl ester (1.22 g, 2.5 mmol) in 4M HCl in dioxane (10 mL) was heated at 70° C. for 2 h. After cooling to RT, the volatiles were concentrated in vacuo and the residue partitioned between DCM and a saturated aqueous solution of NaHCO3. The organic fraction was washed with brine, dried (MgSO4) and then concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-10% MeOH in DCM) to afford the title compound as a colourless oil (639 mg, 68%). LCMS (Method B): RT 2.11 and 2.55 min [M+H]+ 376.2.

1. concentrationthe volatiles were concentrated in vacuo
2. customthe residue partitioned between DCM
3. washThe organic fraction was washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-10% MeOH in DCM)