反应详情

温度

23 °C

A mixture of methyl 1-aminocyclohexanecarboxylate (325 mg, 1.68 mmol), NEt3 (0.49 mL, 3.5 mmol) and 1,4-dichloro-7-isoquinolinesulphonyl chloride (415 mg, 1.40 mmol) in CH2Cl2 (30 mL) was stirred at 23° C. for 16 h. The mixture was diluted with CH2Cl2, washed with dilute HCl (2 M), saturated aqueous NaHCO3, brine, dried (Na2SO4) and evaporated in vacuo. The residue was purified by column chromatography upon silica gel using hexane-EtOAc (80:20 to 70:30) as eluant, followed by trituration with i-Pr2O, to give to give methyl 1-{[(1,4-dichloro-7-isoquinolinyl)sulphonyl]amino}-cyclohexanecarboxylate (132 mg, 0.32 mmol) as a white solid.

1. washwashed with dilute HCl (2 M), saturated aqueous NaHCO3, brine
2. dry with materialdried (Na2SO4)
3. customevaporated in vacuo
4. customThe residue was purified by column chromatography upon silica gel
5. customto give