HRID1719426

反应详情

EQUATION

反应方程式

HRID 1719426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-[2-(4-Benzyloxyphenylamino)-5-methoxyphenyl]ethanone (9 g, 0.0258 mole) in 810 ml of ethanol and 90 ml of acetic acid was hydrogenated in a Parr apparatus in the presence of 900 mg of 10% palladium-on-carbon catalyst. After the required amount of hydrogen had been consumed, the reaction mixture was filtered and the solvents removed in vacuo. The residue was partitioned between ether and 10% aqueous sodium bicarbonate. The ether extracts were dried (MgSO4), the solvent removed, and the residue chromatographed on silica gel using chloroform as the eluant. There was obtained 5.33 g of 1-[2-(4-hydroxyphenylamino)-5-methoxyphenyl]ethanone, orange solid, m.p. 118°-119° C.

WORKUP

后处理

  1. customAfter the required amount of hydrogen had been consumed
  2. filtrationthe reaction mixture was filtered
  3. customthe solvents removed in vacuo
  4. customThe residue was partitioned between ether and 10% aqueous sodium bicarbonate
  5. dry with materialThe ether extracts were dried (MgSO4)
  6. customthe solvent removed
  7. customthe residue chromatographed on silica gel