反应详情

To 4-(2-pyridinyl)benzoic acid (0.0624 g, 0.313 mmol) in DMF (3 mL) was added N-benzyl-N′-cyclohexylcarbodiimide resin (0.294 g, 1.6 mmol/g, 0.47 mmol), 1-hydroxybenzotriazole (0.064 g, 0.47 mmol) and DCM (1 mL) and the mixture was shaken for 30 minutes. 1,1-Dimethylethyl (2S)-2-methyl-4-{[4-(methylamino)phenyl]methyl}-1-piperazine-carboxylate (D3) (100 mg, 0.313 mmol), DMF (3 mL) and DCM (1 mL) were then added and the mixture was shaken for ˜2 days at room temperature The reaction mixture was filtered to remove the resin which was then washed with further DMF/DCM (3:1). The filtrate was concentrated to give the crude product which was purified by column chromatography. Elution with an ether/pentane gradient yielded the title compound (0.055 g). MS (ES): MH+ 501.2.

1. stirringthe mixture was shaken for ˜2 days at room temperature The reaction mixture
2. filtrationwas filtered
3. customto remove the resin which
4. washwas then washed with further DMF/DCM (3:1)
5. concentrationThe filtrate was concentrated
6. customto give the crude product which
7. customwas purified by column chromatography
8. washElution with an ether/pentane gradient