反应详情

温度

0 °C

A solution of 2-nitrobenzenesulfonyl chloride (10.5 g, 47.6 mmol) in anhydrous methylene chloride (25 mL) was added dropwise with stirring to a 0° C. solution of diethanolamine (5.00 g, 47.6 mmol) and triethylamine (4.92 g, 47.6 mmol) in anhydrous methylene chloride (50 mL). Reaction stirred three hours at 0° C. and then overnight at room temperature. Reaction mixture concentrated under reduced pressure. Residue dissolved in ethyl acetate, washed with 1N NaOH, saturated NaHCO3, and brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by normal phase HPLC on a Biotage pre-packed silica gel column eluting with ethyl acetate to afford the title compound. MS (ESI) m/z 291 (M+H)+.

1. customReaction
2. customovernight
3. customat room temperature
4. customReaction mixture
5. concentrationconcentrated under reduced pressure
6. dissolutionResidue dissolved in ethyl acetate
7. washwashed with 1N NaOH, saturated NaHCO3, and brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure
11. customThe residue was purified by normal phase HPLC on a Biotage pre-packed silica gel column
12. washeluting with ethyl acetate