反应详情

A suspension of 1-(4-azidoquinolin-7-ylmethyl)-4-(6-chlorobenzo[b]thiophen-2-sulfonyl)-piperazin-2-one (0.50 g, 1.04 mmol) in 100 mL of acetic acid/methanol (˜1:10) is treated with 10% Pd/C (0.15 g) and stirred under hydrogen for 1.5 hours. The resulting solution is filtered through Celite and the filtrate is evaporated in vacuo. The organic layer is concentrated and the residue is purified by reverse phase HPLC (gradient elution of 30% of 0.1% aqueous TFA/acetonitrile to 100% acetonitrile) and lyopholized to give the title compound (0.39 g, 0.86 mmol). MS (ISP) m/z 487, 489, (M+H), Cl pattern.

1. filtrationThe resulting solution is filtered through Celite
2. customthe filtrate is evaporated in vacuo
3. concentrationThe organic layer is concentrated
4. customthe residue is purified by reverse phase HPLC (gradient elution of 30% of 0.1% aqueous TFA/acetonitrile to 100% acetonitrile)