反应详情

温度

55 °C

A solution of 1.30 g (2.85 mmol) of 1-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-4-[3-(tetrahydro-pyran-2-yloxy)-propyl]-[1,4]diazepan-5-one in 6 ml of methanol was treated with 0.22 g (0.86 mmol) of pyridinium toluene-4-sulfonate and stirred at 55° C. for 30 min. The reaction was cooled and extracted with aqueous 10% KHSO4/Et2O (3×). The organic phases were washed with aqueous saturated NaHCO3, aqueous 10% NaCl, dried (Na2SO4) and evaporated to give after crystallization (Et2O) 0.98 g (92%) of the title compound as white solid.

1. temperatureThe reaction was cooled
2. extractionextracted with aqueous 10% KHSO4/Et2O (3×)
3. washThe organic phases were washed with aqueous saturated NaHCO3, aqueous 10% NaCl
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customto give
7. customafter crystallization (Et2O) 0.98 g (92%) of the title compound as white solid