反应详情

In benzene (30 ml) are dissolved 4-oxo-3,4-dihydro-3-hydroxy-1,2,3-benzotriazine (2.4 g) and triethylamine (2.1 ml) and thereto is added dropwise methanesulfonyl chloride (1.7 g), whereby faint exotherm occurs and crystals are precipitated. The reaction mixture is extracted with ethyl acetate (80 ml). The extract is washed with water, an aqueous sodium hydrogen carbonate and water in order, dried over anhydrous magnesium sulfate and then distilled to remove the solvent. The resulting residue is washed with ether-petroleum ether and dried to give 4-oxo-3,4-dihydro-3-methanesulfonyloxy-1,2,3-benzotriazine (2.6 g), melting point: 132°-134° C. Infrared spectrum: 1720, 1380, 1175 cm-1.

1. customcrystals are precipitated
2. extractionThe reaction mixture is extracted with ethyl acetate (80 ml)
3. washThe extract is washed with water
4. dry with materialan aqueous sodium hydrogen carbonate and water in order, dried over anhydrous magnesium sulfate
5. distillationdistilled
6. customto remove the solvent
7. washThe resulting residue is washed with ether-petroleum ether
8. customdried