HRID2056970

反应详情

EQUATION

反应方程式

HRID 2056970 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dimethyl 1,4-cyclohexanedione-2,5-dicarboxylate (9.12 gm; 40 mmol) and methanol (200 ml) were heated to boiling, then 4-fluoroaniline (8.35 ml (9.78 gm); 42 mmol) was added followed by conc. hydrochloric acid (400 μl). The mixture was refluxed for 3 hours under a nitrogen atmosphere. On cooling a yellow solid precipitated out which was collected by filtration, washed with methanol and dried under vacuum to give 15.8 gm (96%) of dimethyl 2,5-bis{(4-fluorophenyl)amino}cyclohexa-1,4-diene-1,4-dicarboxylate.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 3 hours under a nitrogen atmosphere
  2. temperatureOn cooling a yellow solid
  3. customprecipitated out which
  4. filtrationwas collected by filtration
  5. washwashed with methanol
  6. customdried under vacuum