HRID1704702

反应详情

EQUATION

反应方程式

HRID 1704702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1.5 g. (0.005 mol) of 3,5-bis-methylsulfonamidonitrobenzene in 100 ml. of ethanol and 300 mg. of 10% palladium-on-carbon was hydrogenated in a Parr apparatus until hydrogen uptake had ceased. The catalyst was filtered, the ethanol was removed under reduced pressure and the residue was dissolved in 30 ml. of methanol. This solution of 3,5-bis-methylsulfonamidoaniline (1.36 g.) and 1.06 g. (0.005 mol) of 3,5-diacetyl-4,6-dihydroxy-2H-pyran-2-one was refluxed for two hours under nitrogen. The reaction mixture was filtered to give 5-acetyl-4-hydroxy-3-[1-(3,5-bis-methylsulfonamidophenylamino)ethylidene]-2H-pyran-2,6(3H)-dione, m.p. 260° C.

WORKUP

后处理

  1. additionA mixture of 1.5 g
  2. filtrationThe catalyst was filtered
  3. customthe ethanol was removed under reduced pressure
  4. dissolutionthe residue was dissolved in 30 ml
  5. filtrationThe reaction mixture was filtered