HRID653518

反应详情

EQUATION

反应方程式

HRID 653518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customThe catalyst is removed
  2. customthe solvent evaporated
  3. additionthe residue taken up with a mixture of water and ethyl acetate
  4. customThe organic phase is separated
  5. washwashed with a saturated aqueous solution of sodium chloride
  6. customdried
  7. concentrationconcentrated
  8. customThe residue is crystallised from acetonitrile