反应详情

A stirred mixture of phenyl(5-(tert-butyl)-2-methoxy-3-(methylsulfonamido)phenyl)-carbamate (see step 1(vii) above; 95 mg, 0.239 mmol), the product from step (vi) above (120 mg, 0.217 mmol) and Et3N (6 μL, 0.043 mmol) in i-PrOAc (3 mL) was heated at 70° C. overnight. The reaction was cooled to rt and concentrated in vacuo. The remainder was purified by chromatography on silica gel (40 g column, 0-5% MeOH in EtOAc) to afford an oil, which was triturated with diethyl ether to afford a light beige solid. The crude product was purified by preparative HPLC (Varian, Basic (10 mM Ammonium Bicarbonate), Waters X-Bridge Prep-C18, 5 μm, 19×50 mm column, 35-70% MeCN in Water) to afford the title compound (69 mg) as an off-white solid.

1. concentrationconcentrated in vacuo
2. customThe remainder was purified by chromatography on silica gel (40 g column, 0-5% MeOH in EtOAc)
3. customto afford an oil, which
4. customwas triturated with diethyl ether
5. customto afford a light beige solid
6. customThe crude product was purified by preparative HPLC (Varian, Basic (10 mM Ammonium Bicarbonate), Waters X-Bridge Prep-C18, 5 μm, 19×50 mm column, 35-70% MeCN in Water)