N-[(E)-(2,4,6-trifluorophenyl)methylideneamino]methanamine

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

実験手順: N-Methyl-N′-[1-(2,4,6-trifluoro-phenyl)-meth-(E)-ylidene]-hydrazine (3.85 g, 20.46 mmol) was heated in a seal tube at 210° C. for 2 hours. After cooled to room temperature, the black residue was dissolved in DCM and purified on flash chromatography (EtOAc:Hexane 10:90) to give the title compound as a light yellow crystal (1.926 g, 56%). 1H-NMR (400 MHz, MeOH-d4) δ ppm 8.05 (s, 1H); 7.16 (d, 1H); 6.75 (t, 1H); 3.32 (s, 3H). LCMS (method B): [MH]+=169, tR=2.28 min. purified on flash chromatography (EtOAc:Hexane 10:90)

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

実験手順: A solution of 2,4,6-Trifluoro-benzaldehyde (3 g, 18.74 mmol) and methyl hydrazine (40% in water, 2.6 ml, 18.74 mmol) in 20 ml anhydrous ethanol was stirred at room temperature for 1 hour. Solvent was evaporated to give the title compound as a white solid which was used in the next step without purification (3.95 g, 100%). LCMS (method B): [MH]+=189, tR=2.16 min. Solvent was evaporated

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

実験手順: A solution of 2,4,6-Trifluoro-benzaldehyde (3 g, 18.74 mmol) and methyl hydrazine (40% in water, 2.6 ml, 18.74 mmol) in 20 ml anhydrous ethanol was stirred at room temperature for 1 hour. Solvent was evaporated to give the title compound as a white solid which was used in the next step without purification (3.95 g, 100%). LCMS (method B): [MH]+=189, tR=2.16 min. Solvent was evaporated

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

実験手順: N-Methyl-N′-[1-(2,4,6-trifluoro-phenyl)-meth-(E)-ylidene]-hydrazine (3.85 g, 20.46 mmol) was heated in a sealed tube at 210° C. for 2 h. After cooling, the black residue was dissovled in DCM and purified by flash chromatography (EtOAc:hexane 10:90) to give the title compound as a light yellow crystal (1.926 g, 56%). 1H-NMR (400 MHz, MeOH-d4) δ ppm 8.05 (s, 1H), 7.16 (d, 1H), 6.75 (t, 1H), 3.32 (s, 3H). LCMS (method B): [MH]+=169, tR=2.28 min. After cooling purified by flash chromatography (EtOAc:hexane 10:90)

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

実験手順: A solution of 2,4,6-trifluorobenzaldehyde (3 g, 18.74 mmol) and methyl hydrazine (40% in water, 2.6 mL, 18.74 mmol) in 20 mL of anhydrous ethanol was stirred at rt for 1 h. Solvent was evaporated to give the crude title compound as a white solid which was used in the next step without purification (3.95 g, 100%). LCMS (method B): [MH]+=189, tR=2.16 min. Solvent was evaporated

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

実験手順: N-Methyl-N′-[1-(2,4,6-trifluoro-phenyl)-meth-(E)-ylidene]-hydrazine (3.85 g, 20.46 mmol) was heated in a seaed tube at 210° C. for 2 h. After cooling, the black residue was dissovled in DCM and purified by flash chromatography (EtOAc:hexane 10:90) to give the title compound as a light yellow crystal (1.926 g, 56%). 1H-NMR (400 MHz, MeOH-d4) δ ppm 8.05 (s, 1H), 7.16 (d, 1H), 6.75 (t, 1H), 3.32 (s, 3H). LCMS (method B): [MH]+=169, tR=2.28 min. After cooling purified by flash chromatography (EtOAc:hexane 10:90)

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

実験手順: A solution of 2,4,6-trifluorobenzaldehyde (3 g, 18.74 mmol) and methyl hydrazine (40% in water, 2.6 mL, 18.74 mmol) in 20 mL of anhydrous ethanol was stirred at rt for 1 h. Solvent was evaporated to give the crude title compound as a white solid which was used in the next step without purification (3.95 g, 100%). LCMS (method B): [MH]+=189, tR=2.16 min. Solvent was evaporated

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

実験手順: N-Methyl-N′-[1-(2,4,6-trifluoro-phenyl)-meth-(E)-ylidene]-hydrazine (3.85 g, 20.46 mmol) was heated in a seal tube at 210° C. for 2 hours. After cooled to room temperature, the black residue was dissolved in DCM and purified on flash chromatography (EtOAc:Hexane 10:90) to give the title compound as a light yellow crystal (1.926 g, 56%). 1H-NMR (400 MHz, MeOH-d4) δ ppm 8.05 (s, 1H); 7.16 (d, 1H); 6.75 (t, 1H); 3.32 (s, 3H). LCMS (method B): [MH]+=169, tR=2.28 min. purified on flash chromatography (EtOAc:Hexane 10:90)

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

実験手順: A solution of 2,4,6-Trifluoro-benzaldehyde (3 g, 18.74 mmol) and methyl hydrazine (40% in water, 2.6 ml, 18.74 mmol) in 20 ml anhydrous ethanol was stirred at room temperature for 1 hour. Solvent was evaporated to give the title compound as a white solid which was used in the next step without purification (3.95 g, 100%). LCMS (method B): [MH]+=189, tR=2.16 min. Solvent was evaporated