反应详情

温度

70 °C

A mixture of (RS)-5-[5-(benzhydrylidene-amino)-2-fluoro-phenyl]-5-cyclopropyl-morpholin-3-one (2.10 g, 5.07 mmol) and Lawesson's reagent (0.926 mg, 2.3 mmol) in tetrahydrofuran (15 mL) was stirred at 70° C. for 3 hours. For the workup, the reaction mixture was diluted with ethyl acetate and extracted with a saturated solution of sodium hydrogen-carbonate. The organic layer was dried over sodium sulfate and evaporated. The crude product was purified by chromatography on silica gel using a gradient of hexane/ethyl acetate as the eluent. The (RS)-5-[5-(benzhydrylidene-amino)-2-fluoro-phenyl]-5-cyclopropyl-morpholine-3-thione was obtained as a yellow foam (1.42 g, 65% of theory). Mass (calculated) C26H23FN2OS [430.545]; (found) [M+H]+=431.

1. extractionextracted with a saturated solution of sodium hydrogen-carbonate
2. dry with materialThe organic layer was dried over sodium sulfate
3. customevaporated
4. customThe crude product was purified by chromatography on silica gel using a gradient of hexane/ethyl acetate as the eluent