反应详情

To a solution of 1-[1-(toluene-4-sulfonyl)-1H-pyrazol-3-yl]-propan-1-one (2.10 g, 7.55 mmol) in dichloroethane was added (R)-(+)-2-methyl-2-propanesulfinamide (1.45 g, 12.00 mmol) and titanium (IV) isopropoxide (4.26 g, 15.00 mmol) and the mixture was warmed at reflux overnight. After cooling, the solvent was concentrated in vacuo. The residue was diluted with EtOAc and saturated aqueous NaCl was added dropwise. After 20 minutes, the solution was passed through diatomaceous earth. The combined organics were washed with brine and dried over sodium sulfate. The solvent was concentrated in vacuo to afford 2-methyl-propane-2-sulfinic acid [1-[1-(toluene-4-sulfonyl)-1H-pyrazol-3-yl]-prop-(E)-ylidene]-amide.

1. temperaturethe mixture was warmed
2. temperatureat reflux overnight
3. temperatureAfter cooling
4. concentrationthe solvent was concentrated in vacuo
5. additionThe residue was diluted with EtOAc and saturated aqueous NaCl
6. additionwas added dropwise
7. washThe combined organics were washed with brine
8. dry with materialdried over sodium sulfate
9. concentrationThe solvent was concentrated in vacuo