Water → HCID 18670459, compound

Participants

Reaction Steps

100 ml of a solution of 7.0 g of ethyl 10H-pyrazino[2,3-b][1,4]benzothiazine-7-carboxylate in N,N-dimethylformamide was ice-cooled in a nitrogen atmosphere and 1.3 g of sodium hydride (60% oily) was added thereto. Then the resulting mixture was brought back to room temperature and stirred for 1 hour. Next, it was ice-cooled again and 2.5 ml of chloromethyl ether was dropped thereinto. After the completion of the reaction, the reaction mixture was distributed into water and ethyl acetate. The organic layer was extracted, 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 ethyl acetate/hexane) to thereby give 5.0 g of ethyl 10-(methoxymethyl)-10H-pyrazino[2,3-b][1,4]benzothiazine-7-carboxylate as pale yellow crystals.

Provenance & Evidence