HRID15716

反应详情

EQUATION

反应方程式

HRID 15716 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,4-Diethoxy-2,3-naphthalenedicarboxylic anhydride (23.3 g, 81.5 mmol) and ethyl (4-aminophenyl)acetate (14.8 g, 82 mmol) were refluxed under nitrogen in acetic acid (160 ml) overnight. The mixture was cooled to room temperature and poured into water (1 L). The white solid was filtered, washed with water and dissolved in dichloromethane (800 ml). The solution was washed with water, brine and dried (MgSO4) and the solvent evaporated under vacuum to give ethyl[4-(4,9-diethoxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate as an off-white solid, 33 g, 96%.

WORKUP

后处理

  1. filtrationThe white solid was filtered
  2. washwashed with water
  3. dissolutiondissolved in dichloromethane (800 ml)
  4. washThe solution was washed with water, brine
  5. dry with materialdried (MgSO4)
  6. customthe solvent evaporated under vacuum