Hydrochloric Acid → HCID 11207166, compound

Participants

Reaction Steps

A solution of 21.5 g of the product obtained in step A) and 13.4 g of iron powder in a mixture of 25 ml of water and 25 ml of ethanol is brought to the reflux point. A solution of 50 ml of concentrated hydrochloric acid in a mixture of 34 ml of water and 34 ml of ethanol is then added slowly. Reflux is maintained for 2 hours. The reaction medium is then poured onto ice, treated with a saturated solution of NaHCO3 and then extracted with DCM, washed with water and dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica using DCM as the eluent. 7.2 g of the expected product are obtained after crystallization from heptane. M.p.=62° C.

Provenance & Evidence