反应 #1289112
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09073890B2
反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a dry reaction vial was added cyclohexylamine (40 uμmol, 1.0 eq) and PS-carbodiimide resin (72 μmol, 1.8 eq). The solution of 2-amino-benzoic acid (44 μmol, 1.1 eq), diisopropyl ethyl amine (10 μLl) and HOBt (44 μmol, 1.1 eq) in THF (500 μL) was added to the above vial. The reaction mixture was heated at 40° C. for 6 h on a shaker. The resin was removed by filtration and washed with 10% MeOH/CH2Cl2. The solvent was removed in vacuo and the residue was applied to solid phase extraction cartridge (basic silica, 200 mg) and eluted with 50% EtOAc/CH2Cl2. After removal of the solvents, the crude 2-amino-N-cyclohexyl-benzamide was obtained and used for the following reaction. To a dry reaction The resin was removed by filtration washed with 10% MeOH/CH2Cl2 The solvent was removed in vacuo the residue was applied to solid phase extraction cartridge (basic silica, 200 mg) eluted with 50% EtOAc/CH2Cl2 After removal of the solvents
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