反应详情

To a solution of 2-cyclobutoxy-3-methyl-benzoic acid (400 mg, 1.94 mmol), 2-amino-5-fluoro-indan-2-carboxylic acid ethyl ester (523 mg, 2.33 mmol), HATU (1.11 g, 2.91 mmol) in anhydrous DMF (18 mL) is added DIPEA (480 μL, 2.91 mmol). The resulting solution is stirred at RT overnight. After the removal of DMF in vacuo, the residue is dissolved in EtOAc (100 mL) and washed with water (1×10 mL) and brine (2×10 mL). The organic layer is dried over anhydrous Na2SO4 and concentrated in vacuo. The residue is purified by flash column chromatography (115 g silica gel, gradient elution: 5%-40% EtOAc in heptane) to give a pure product (102) as white solid (681 mg, 85%).

1. customAfter the removal of DMF in vacuo
2. dissolutionthe residue is dissolved in EtOAc (100 mL)
3. washwashed with water (1×10 mL) and brine (2×10 mL)
4. dry with materialThe organic layer is dried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue is purified by flash column chromatography (115 g silica gel, gradient elution: 5%-40% EtOAc in heptane)