反应详情

温度

0 °C

Triphosgene (28 mg, 1/3 equiv) was dissolved in 1 mL of THF and the solution cooled to 0° C. A solution of 4-amino-N-(2-benzoylphenyl)benzenesulfonamide (100 mg) in 3 mL of THF and 0.15 mL of triethylamine was added therto, and the reaction mixture was warmed to rt and stirred for 30 minutes. A solution of tetrahyhdrofurfuryl alcohol (44 mg, 1.5 equiv) in 3 mL of THF and 0.15 mL of triethylamine was added thereto and the reaction mixture was left stirring overnight. The reaction was quenched with water and diluted with EtOAc. The organic layer was washed once each with water and brine, dried over sodium sulfate, filtered, and concentrated in vacuo. The title product was obtained following flash chromatography (10% to 95% EtOAc/hexanes). ESMS, M+H+ found: 481.8.

1. temperaturewas warmed to rt
2. waitthe reaction mixture was left
3. stirringstirring overnight
4. customThe reaction was quenched with water
5. additiondiluted with EtOAc
6. washThe organic layer was washed once each with water and brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo