Hydrochloric Acid → HCID 21245053, compound

Participants

Reaction Conditions

Reaction Steps

15 g of the compound prepared in Example 3, dissolved in 35 ml of tetrahydrofuran, were added under a nitrogen atmosphere to a reactor containing a suspension of 4.95 g of sodium borohydride in 100 ml of tetrahydrofuran, the temperature being maintained at 0° C. 29.6 ml of boron trifluoride etherate in 39 ml of tetrahydrofuran were then added dropwise. After the reaction medium had been allowed to return to room temperature, 69 ml of 10% strength hydrochloric acid were added. The solvent was then removed by distillation at atmospheric pressure, and the residue cooled and then alkalinized with caustic soda solution and then extracted with methylene chloride. After drying and evaporation of the solvent, the product was distilled, and then purified by preparative liquid chromatography on silica gel, using as solvent 2% strength and then 4% strength methanol in dichloromethane.

Provenance & Evidence