HCID 67916224, compound → HCID 67946049, compound

Participants

Reaction Steps

A solution of the product from Example 19 (0.70 g, 1.74 mmol) in 20 mL of methanol and 0.5 mL acetic acid was treated with zinc dust (1.58 g, 320 mesh) and the resulting suspension stirred at room temperature for three hours. The reaction mixture was filtered and the filtrate concentrated. The residue was dissolved in ether (30 mL) and extracted with aqueous 1N HCl (3×15 mL). The combined acid extracts are made basic (pH=11) with potassium carbonate and the resulting aqueous solution was extracted with CH2Cl2 (5×15 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The residue (0.30 g) was converted to its HCl salt by dissolution in ether and treatment with a saturated solution of HCl (gas) in ether. The solid which formed was collected by filtration and dried under vacuum (100° C.) to give the title compound (0.25 g, 54%) as a white solid mp >270° C.

Provenance & Evidence