N-甲基苯甲酰肼

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1.14 g. of o-toluimidic acid ethyl ester, 1.14 g. of 1-methyl-1-benzoylhydrazine and 0.1 g. of o-toluimidic acid ester hydrochloride, as a catalyst, is heated at about 100° C. for three hours under reduced pressure (about 200 mm Hg) and then at about 120° C. for five hours. The raw material is taken up with diethyl ether and the organic solution is washed with aqueous sodium bicarbonate and then dried over Na2SO4. After evaporation of the solvent, the product is distilled at 170° C./0.1 mm Hg. Yield 32%. A mixture of 1.14 g the organic solution is washed with aqueous sodium bicarbonate dried over Na2SO4 After evaporation of the solvent the product is distilled at 170° C./0.1 mm Hg

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of N-methylbenzohydrazide (450 mg, 3.0 mmol) and the Woollins' Reagent (540 mg, 1 mmol) in anhydrous toluene (10 ml), was heated at 120° C. for Ih. The resulting orange solution was cooled to room temperature, the solvent was removed in vacuo and the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc) and to give N-methylbenzoselenohydrazide (415 mg) in 65% yield. the solvent was removed in vacuo the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of N-methylbenzohydrazide (450 mg, 3.0 mmol) and the Woollins' Reagent (540 mg, 1 mmol) in anhydrous toluene (10 ml), was heated at 120° C. for Ih. The resulting orange solution was cooled to room temperature, the solvent was removed in vacuo and the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc) and to give N-methylbenzoselenohydrazide (415 mg) in 65% yield. the solvent was removed in vacuo the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1.14 g. of o-toluimidic acid ethyl ester, 1.14 g. of 1-methyl-1-benzoylhydrazine and 0.1 g. of o-toluimidic acid ester hydrochloride, as a catalyst, is heated at about 100° C. for three hours under reduced pressure (about 200 mm Hg) and then at about 120° C. for five hours. The raw material is taken up with diethyl ether and the organic solution is washed with aqueous sodium bicarbonate and then dried over Na2SO4. After evaporation of the solvent, the product is distilled at 170° C./0.1 mm Hg. Yield 32%. A mixture of 1.14 g the organic solution is washed with aqueous sodium bicarbonate dried over Na2SO4 After evaporation of the solvent the product is distilled at 170° C./0.1 mm Hg

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1.14 g. of o-toluimidic acid ethyl ester, 1.14 g. of 1-methyl-1-benzoylhydrazine and 0.1 g. of o-toluimidic acid ester hydrochloride, as a catalyst, is heated at about 100° C. for three hours under reduced pressure (about 200 mm Hg) and then at about 120° C. for five hours. The raw material is taken up with diethyl ether and the organic solution is washed with aqueous sodium bicarbonate and then dried over Na2SO4. After evaporation of the solvent, the product is distilled at 170° C./0.1 mm Hg. Yield 32%. A mixture of 1.14 g the organic solution is washed with aqueous sodium bicarbonate dried over Na2SO4 After evaporation of the solvent the product is distilled at 170° C./0.1 mm Hg

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methylhydrazine (0.212 ml, 4.0 mmol) was dissolved in dichloromethane (10 ml) and was treated dropwise with benzoylchloride (0.232 ml, 2.0 mmol) in dichloromethane (5 ml). After stirring for 0.5h the solution was evaporated to dryness. The residue was partitioned between water and ethyl acetate. The organic phase was dried and evaporated under reduced pressure to give the title compound (0.20 g, 65%); δH (CDCl3) 3.13 (3H, s), 4.5 (2H, brs), and 7.30 (5H, s). was evaporated to dryness The residue was partitioned between water and ethyl acetate The organic phase was dried evaporated under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of N-methylbenzohydrazide (450 mg, 3.0 mmol) and the Woollins' Reagent (540 mg, 1 mmol) in anhydrous toluene (10 ml), was heated at 120° C. for 1 h. The resulting orange solution was cooled to room temperature, the solvent was removed in vacuo and the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc) and to give N-methylbenzoselenohydrazide (415 mg) in 65% yield. the solvent was removed in vacuo the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1.14 g. of o-toluimidic acid ethyl ester, 1.14 g. of 1-methyl-1-benzoylhydrazine and 0.1 g. of o-toluimidic acid ester hydrochloride, as a catalyst, is heated at about 100° C for 3 hours under reduced pressure (about 200 mm Hg) and then at about 120° C for 5 hours. The raw material is taken up with diethyl ether and the organic solution is washed with aqueous sodium bicarbonate and then dried over Na2SO4. After evaporation of the solvent, the product is distilled at 170° C/0.1 mm Hg. Yield 32%. A mixture of 1.14 g the organic solution is washed with aqueous sodium bicarbonate dried over Na2SO4 After evaporation of the solvent the product is distilled at 170° C/0.1 mm Hg

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of N-methylbenzohydrazide (450 mg, 3.0 mmol) and the Woollins' Reagent (540 mg, 1 mmol) in anhydrous toluene (10 ml), was heated at 120° C. for Ih. The resulting orange solution was cooled to room temperature, the solvent was removed in vacuo and the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc) and to give N-methylbenzoselenohydrazide (415 mg) in 65% yield. the solvent was removed in vacuo the selenoamide purified by column chromatography on silica gel (3:1 Hexane:EtOAc)