反应详情

A mixture of 8-(2,6-dichloro-3,5-dimethoxy-phenyl)quinoxaline-5-carboxylic acid (Step 1.1) (0.400 g, 1.06 mmol), 1-(2-trimethylsilanyl-ethoxymethyl)-1H-imidazol-2-ylamine (Step 14.2) (0.270 g, 1.27 mmol, 1.2 equiv), TBTU (408 mg, 1.27 mmol, 1.2 equiv), DIEA (0.74 mL, 4.23 mmol, 4.0 equiv) in DMF (5 mL) was stirred for 2 h at rt, diluted with EtOAc and H2O, and extracted with EtOAc.washed with a saturated aqueous solution of NaHCO3, H2O, and brine. The organic phase was washed with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH, 95:5) to afford 0.518 g of the title compound as a yellow foam: ES-MS: 573.8/575.8 [M+H]+; tR=5.03 min (System 1); Rf=0.19 (DCM2/MeOH, 95:5).

1. extractionextracted with EtOAc
2. washwashed with a saturated aqueous solution of NaHCO3, H2O, and brine
3. washThe organic phase was washed with H2O and brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography (DCM/MeOH, 95:5)