Water → HCID 18670347, compound

Participants

Reaction Steps

To 5 ml of a solution of 350 mg of ammonium thiocyanate in acetone was added in a nitrogen atmosphere 0.50 ml of benzoyl chloride and the resulting mixture was heated under reflux for 5 minutes. Then 5 ml of a solution of 890 mg of 8-aminomethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine in acetone was added thereto and the resulting mixture was heated under reflux for additional 1.5 hours. Next, the reaction mixture was distributed into water and ethyl acetate, washed with water and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with n-hexane/ethyl acetate) and recrystallized from diisopropyl ether to thereby give 710 mg of the title compound as yellow crystals.

Provenance & Evidence