HRID653518
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2,2 g of 6-bromo-3,4-dihydro-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide are hydrogenated in the presence of 0.7 g of sodium acetate and 0.3 g of 5% palladium on carbon catalyst at 20° C. and 1 bar in 45 ml of tetrahydrofurane. The catalyst is removed, the solvent evaporated, the residue taken up with a mixture of water and ethyl acetate. The organic phase is separated, washed with a saturated aqueous solution of sodium chloride, dried and concentrated. The residue is crystallised from acetonitrile, affording 3,4-dihydro-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide with a melting point of 204°-205° C.
WORKUP
后处理
- customThe catalyst is removed
- customthe solvent evaporated
- additionthe residue taken up with a mixture of water and ethyl acetate
- customThe organic phase is separated
- washwashed with a saturated aqueous solution of sodium chloride
- customdried
- concentrationconcentrated
- customThe residue is crystallised from acetonitrile