N-(3-chloro-4-fluorophenyl)formamide

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: 17.5 g of sodium hydride (57% in mineral oil) was added, in portions, to a stirred solution of 55.5 g of 1A and 71 g of methyl iodide in 250 ml of tetrahydrofuran at room temperature. The resulting mixture was stirred and refluxed for 2 hours, poured into ice water and filtered. The solid was washed with water, dried and recrystallized from hexane to give N-(3-chloro-4-fluorophenyl)N-methylformamide (5A), as a white crystalline solid, mp: 47°-48° C. refluxed for 2 hours filtered The solid was washed with water dried recrystallized from hexane

反応条件: temp:106.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 100 g of 3-chloro-4-fluoroaniline and 400 ml of 97% formic acid was refluxed (106° C.) for three hours. The mixture then was poured into ice water and the resulting mixture was filtered. The solid was washed with water and dried to give N-(3-chloro-4-fluorophenyl)formamide (J. Org. Chem., 26, 2563 (1961)) (1A), as a colorless crystalline solid, mp: 94°-97° C. the resulting mixture was filtered The solid was washed with water dried

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

実験手順: 17.5 g of sodium hydride (57% in mineral oil) was added, in portions, to a stirred solution of 55.5 g of 1A and 71 g of methyl iodide in 250 ml of tetrahydrofuran at room temperature. The resulting mixture was stirred and refluxed for 2 hours, poured into ice water and filtered. The solid was washed with water, dried and recrystallized from hexane to give N-(3-chloro-4-fluorophenyl)N-methylformamide (5A), as a white crystalline solid, mp: 47°-48° C. refluxed for 2 hours filtered The solid was washed with water dried recrystallized from hexane

反応条件: temp:106.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 100 g of 3-chloro-4-fluoroaniline and 400 ml of 97% formic acid was refluxed (106° C.) for three hours. The mixture then was poured into ice water and the resulting mixture was filtered. The solid was washed with water and dried to give N-(3-chloro-4-fluorophenyl)formamide (J. Org. Chem., 26, 2563 (1961)) (1A), as a colorless crystalline solid, mp: 94°-97° C. the resulting mixture was filtered The solid was washed with water dried

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: 17.5 g of sodium hydride (57% in mineral oil) was added, in portions, to a stirred solution of 55.5 g of 1A and 71 g of methyl iodide in 250 ml of tetrahydrofuran at room temperature. The resulting mixture was stirred and refluxed for 2 hours, poured into ice water and filtered. The solid was washed with water, dried and recrystallized from hexane to give N-(3-chloro-4-fluorophenyl)N-methylformamide (5A), as a white crystalline solid, mp: 47°-48° C. refluxed for 2 hours filtered The solid was washed with water dried recrystallized from hexane

反応条件: temp:106.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 100 g of 3-chloro-4-fluoroaniline and 400 ml of 97% formic acid was refluxed (106° C.) for three hours. The mixture then was poured into ice water and the resulting mixture was filtered. The solid was washed with water and dried to give N-(3-chloro-4-fluorophenyl)formamide (J. Org. Chem., 26, 2563 (1961)) (1A), as a colorless crystalline solid, mp: 94°-97° C. the resulting mixture was filtered The solid was washed with water dried