1-methyl-2-nitrosobenzene

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: DBU (15 mg, 0.1 mmol) was added under argon to a solution of benzaldehyde (106 mg, 1 mmol), 1-methyl-2-nitrosobenzene (121 mg, 1 mmol) and catalyst (36.4 mg, 0.1 mmol) in dichloromethane (5 ml). The reaction mixture was stirred at room temperature for 60 min. The solvent was removed under vacuum, and the residue was purified by flash silica gel column chromatography using hexane and ethyl acetate as the eluents. The solvent was removed under vacuum the residue was purified by flash silica gel column chromatography

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

実験手順: 2.4 Parts of o-nitrosotoluene and 4.1 parts of diphenylcyclopropenone in 50 parts of tetrahydrofuran is heated at the reflux temperature for 48 hours. Solvent then is removed under reduced pressure and the residue is crystallized from cyclohexane. Recrystallization from ethanol gives, as red granules, 2-(o-tolyl)-3,4-diphenylisoxazolin-5-one, melting at about 142°-143° C. That compound is represented structurally by the following formula. ##STR6## Solvent then is removed under reduced pressure the residue is crystallized from cyclohexane Recrystallization from ethanol

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

実験手順: 4.982 g of 97% ortho-nitrosotoluene (41.12 mmol) were dissolved in 20 ml of methylene chloride at room temperature and 5.93 g of 98% methane sulfonic acid (61.7 mmol = molar ratio of 1:1.5) added thereto in the course of 2 minutes. Stirring was continued for one-half hour at room temperature and subsequently the dark brown, clear solution sprayed into water of 30° C. under a vacuum, whereby the methylene chloride was distilled off simultaneously. By means of filtration, it was possible to obtain 4.85 g = 97% of theoretical, of N-(2-methylphenyl)-N-(3-methyl-4-nitrosophenyl)-hydroxylamine in the form of a light yellow powder. in the course of 2 minutes was continued for one-half hour at room temperature was distilled off simultaneously By means of filtration, it

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: 4.982 g of 97% ortho-nitrosotoluene (41.12 mmol) were dissolved in 20 ml of methylene chloride at room temperature and 5.93 g of 98% methane sulfonic acid (61.7 mmol = molar ratio of 1:1.5) added thereto in the course of 2 minutes. Stirring was continued for one-half hour at room temperature and subsequently the dark brown, clear solution sprayed into water of 30° C. under a vacuum, whereby the methylene chloride was distilled off simultaneously. By means of filtration, it was possible to obtain 4.85 g = 97% of theoretical, of N-(2-methylphenyl)-N-(3-methyl-4-nitrosophenyl)-hydroxylamine in the form of a light yellow powder. in the course of 2 minutes was continued for one-half hour at room temperature was distilled off simultaneously By means of filtration, it

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

実験手順: DBU (15 mg, 0.1 mmol) was added under argon to a solution of benzaldehyde (106 mg, 1 mmol), 1-methyl-2-nitrosobenzene (121 mg, 1 mmol) and catalyst (36.4 mg, 0.1 mmol) in dichloromethane (5 ml). The reaction mixture was stirred at room temperature for 60 min. The solvent was removed under vacuum, and the residue was purified by flash silica gel column chromatography using hexane and ethyl acetate as the eluents. The solvent was removed under vacuum the residue was purified by flash silica gel column chromatography

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

実験手順: 2.4 Parts of o-nitrosotoluene and 4.1 parts of diphenylcyclopropenone in 50 parts of tetrahydrofuran is heated at the reflux temperature for 48 hours. Solvent then is removed under reduced pressure and the residue is crystallized from cyclohexane. Recrystallization from ethanol gives, as red granules, 2-(o-tolyl)-3,4-diphenylisoxazolin-5-one, melting at about 142°-143° C. That compound is represented structurally by the following formula. ##STR6## Solvent then is removed under reduced pressure the residue is crystallized from cyclohexane Recrystallization from ethanol

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: 4.982 g of 97% ortho-nitrosotoluene (41.12 mmol) were dissolved in 20 ml of methylene chloride at room temperature and 5.93 g of 98% methane sulfonic acid (61.7 mmol = molar ratio of 1:1.5) added thereto in the course of 2 minutes. Stirring was continued for one-half hour at room temperature and subsequently the dark brown, clear solution sprayed into water of 30° C. under a vacuum, whereby the methylene chloride was distilled off simultaneously. By means of filtration, it was possible to obtain 4.85 g = 97% of theoretical, of N-(2-methylphenyl)-N-(3-methyl-4-nitrosophenyl)-hydroxylamine in the form of a light yellow powder. in the course of 2 minutes was continued for one-half hour at room temperature was distilled off simultaneously By means of filtration, it