(Diethylamino)sulfur trifluoride → HCID 59822033, compound

Participants

Reaction Steps

At −55° C. and under argon, 3.21 ml of diethylaminosulphur trifluoride (24.3 mmol, 1.5 eq.) are added dropwise to a solution of 9.96 g (16.2 mmol) of the compound from Example 5A in 300 ml of dry toluene. The mixture is stirred at this temperature for 1 h and then at room temperature for a further 2 h. For work-up, 120 ml of a saturated sodium bicarbonate solution are added carefully. The mixture is extracted three times in total with ethyl acetate. The combined organic phases are washed with saturated sodium chloride solution, dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude product is purified by filtration through silica gel (mobile phase: cyclohexane/ethyl acetate 9:1).

Provenance & Evidence