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 1 N 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 1 N 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