HRID2056970
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was refluxed for 3 hours under a nitrogen atmosphere
- temperatureOn cooling a yellow solid
- customprecipitated out which
- filtrationwas collected by filtration
- washwashed with methanol
- customdried under vacuum