Sodium Bicarbonate → HCID 69105088, compound

Participants

Reaction Steps

A solution of 33.1 g of steroid 3 in 400 ml of THF was cooled to 0° C., mixed in portions with 51.0 g of LTBAH, and the solution was stirred for 1 hour while cooling was continued and for 1 hour at room temperature. 25 ml of saturated sodium bicarbonate solution was added in drops to the reaction solution at 0° C., the precipitate that was produced was separated by filtration on Celite, and the filtrate was concentrated by evaporation to a very large extent. The residue was extracted several times with ethyl acetate, the collected organic phases were then washed with brine, dried on magnesium sulfate, and the solvent was removed in a vacuum. In this way, 27.6 g (97%) of foamy 4 was obtained, which was used without further purification in the next stage.

Provenance & Evidence