反应详情

温度

130 °C

To 1,1-dimethylethyl (2S)-4-({6-[[(6-chloro-3-pyridinyl)carbonyl](methyl)amino]-3-pyridinyl}methyl)-2-methyl-1-piperazinecarboxylate (D106) (0.139 g, 0.303 mmol) in DMF (4 mL) under an argon atmosphere was added potassium carbonate (0.293 g, 0.212 mmol) and 4-fluorophenol (0.169 g, 1.51 mmol). The reaction mixture was stirred and heated at 130° C. for 5 h then concentrated in vacuo. The residue was re-dissolved in DCM/water. The organic layer was washed with 2M NaOH solution and brine then dried (Na2SO4) and concentrated to give the crude product which was purified by column chromatography. Elution with EtOAc/DCM gave the title compound as a colourless oil (0.054 g). MS (ES): MH+ 536.2.

1. concentrationthen concentrated in vacuo
2. dissolutionThe residue was re-dissolved in DCM/water
3. washThe organic layer was washed with 2M NaOH solution and brine
4. dry with materialthen dried (Na2SO4)
5. concentrationconcentrated
6. customto give the crude product which
7. customwas purified by column chromatography
8. washElution with EtOAc/DCM