反应详情

温度

0 °C

Compound 2 (150 mg, 0.41 mmol) was dissolved in DCM and cooled to 0° C. Ethanesulfonyl chloride (62.2 mg, 0.49 mmol) was added, followed by DIEA (0.21 mL, 1.22 mmol). The reaction mixture was allowed to warm to ambient temperature and stirred overnight. The mixture was diluted with DCM and washed with saturated NaHCO3 solution. The organic layer was separated, washed with brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by normal phase chromatography eluting with 10-50% methanol/DCM gradient to provide Compound 91 as a white solid (0.13 g, 69%). MS: m/z 462.34 [M+H]+.

1. temperatureto warm to ambient temperature
2. washwashed with saturated NaHCO3 solution
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated
7. customThe residue was purified by normal phase chromatography
8. washeluting with 10-50% methanol/DCM gradient