反应详情

温度

5 °C

A solution of the title B compound, 4-[5-(2,4-dimethoxy-benzyl)-1,1,4-trioxo-1,2,5-thiadiazolidin-2-ylmethyl]-benzoic acid (84 mg, 0.2 mmol) and 4-hydroxymethyl-benzoic acid t-butyl ester (42 mg, 0.2 mmol) in CH2Cl2 (3 mL) is treated with DMAP (12 mg, 0.1 mmol) and the reaction is cooled to 5° C. EDCl (39 mg, 0.2 mmol) is then added and the reaction is stirred for 16 h. The mixture is concentrated and partioned between EtOAc and 1N aqueous HCl. The organic solution is washed with saturated aqueous NaHCO3 and brine, dried over anhydrous MgSO4 and concentrated to give 4-(1,1,4-trioxo-1,2,5-thiadiazolidin-2-ylmethyl)-benzoic acid 4-t-butoxycarbonyl-benzyl ester as a white solid.

1. concentrationThe mixture is concentrated
2. washThe organic solution is washed with saturated aqueous NaHCO3 and brine
3. dry with materialdried over anhydrous MgSO4
4. concentrationconcentrated