3,4-dichloro-1-(4-fluorophenyl)pyrrole-2,5-dione

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 15g (0.07 mol) of dimethyl 2,3-dichloromaleate was added to 100 ml of water. To the resulting solution 6.7g (0.06 mol) of 4-fluoroaniline was added dropwise over a period of 5 min. at reflux temperatures under agitation. The mixture was then allowed to react for 2 hours at reflux temperatures. Upon cooling the reaction mixture, precipitated crystal was separated by filtration to obtain 15.2g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 240°-242° C (not corrected) at a yield of 97.3%. An analysis by gas chromatography showed the product had a purity of 94.1%. at reflux temperatures under agitation to react for 2 hours at reflux temperatures Upon cooling the reaction mixture precipitated crystal was separated by filtration

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18.5g (0.1 mol) of 2,3-dichloromaleic acid was dissolved in 120 ml of water. To the resulting solution 8.9g (0.08mol) of 4-fluoroaniline was added dropwise over a period of 5 min. at reflux temperatures under agitation. The mixture was then allowed to react for 2 hours at reflux temperatures. Upon cooling the reaction mixture, precipitated crystal was separated by filtration to obtain 20.3g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 239°-240° C (not corrected) at a yield of 98.1%. An analysis by gas chromatography showed the product had a purity of 95.5%. at reflux temperatures under agitation to react for 2 hours at reflux temperatures Upon cooling the reaction mixture precipitated crystal was separated by filtration

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18.5g (0.1 mol) of 2,3-dichloromaleic acid was dissolved in 120 ml of water. To the resulting solution 8.9g (0.08mol) of 4-fluoroaniline was added dropwise over a period of 5 min. at reflux temperatures under agitation. The mixture was then allowed to react for 2 hours at reflux temperatures. Upon cooling the reaction mixture, precipitated crystal was separated by filtration to obtain 20.3g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 239°-240° C (not corrected) at a yield of 98.1%. An analysis by gas chromatography showed the product had a purity of 95.5%. at reflux temperatures under agitation to react for 2 hours at reflux temperatures Upon cooling the reaction mixture precipitated crystal was separated by filtration

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.56g of the thusly resulted 4-fluoroanilinium 2,3-dichloromaleate was suspended in 40 ml of water and allowed to react for 2 hours at reflux temperatures. Upon cooling the reaction mixture, precipitated crystal was separated by filtration to obtain 4.8g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 240°-242° C (not corrected) at a yield of 95.0%. An analysis by gas chromatography showed the product had a purity of 99.2%. to react for 2 hours at reflux temperatures Upon cooling the reaction mixture precipitated crystal was separated by filtration

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.55g (0.05 mol) of 4-fluoroaniline was emulsified in 150 ml of water. Then to the resulting emulsion 10g (0.06 mol) of 2,3-dichloromaleic anhydride in 50 ml of water was added dropwise over a period of 30 min. at room temperatures under agitation. The mixture was then allowed to react at reflux temperatures. Upon cooling the reaction mixture, a crystal was removed out, which was separated by filtration to obtain 12.9g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 240°-243° C (not corrected) at a yield of 99.1%. An analysis by gas chromatography showed the product had a purity of 98.6%. to react at reflux temperatures Upon cooling the reaction mixture a crystal was removed out which was separated by filtration

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.55g (0.05 mol) of 4-fluoroaniline was emulsified in 150 ml of water. Then to the resulting emulsion 10g (0.06 mol) of 2,3-dichloromaleic anhydride in 50 ml of water was added dropwise over a period of 30 min. at room temperatures under agitation. The mixture was then allowed to react at reflux temperatures. Upon cooling the reaction mixture, a crystal was removed out, which was separated by filtration to obtain 12.9g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 240°-243° C (not corrected) at a yield of 99.1%. An analysis by gas chromatography showed the product had a purity of 98.6%. to react at reflux temperatures Upon cooling the reaction mixture a crystal was removed out which was separated by filtration

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10g (0.06 mol) of 2,3-dichloromaleic anhydride was dissolved in 200 ml of water. Then to the resulting solution 5.55g (0.05 mol) of 4-fluoroaniline was added dropwise over a period of 5 min. at room temperature under agitation. The mixture was then allowed to react for 2 hours at reflux temperatures. Upon cooling the reaction mixture, precipitated crystal was separated by filtration to obtain 12.9g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 240°-243° C (not corrected) at a yield of 99.2%. An anaylsis by gas chromatography showed the product had a purity of 99.3%. to react for 2 hours at reflux temperatures Upon cooling the reaction mixture precipitated crystal was separated by filtration