1-benzamido-3-methylthiourea

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: A stirred mixture of 1-benzoyl-4-methylthiosemicarbazide (20.9 g, 1.00×10-1 mole) and 1 molar aqueous NaHCO3 (1000 ml, 1 mole) was heated to reflux. After refluxing overnight the reaction was cooled in an ice bath. With stirring the solution was carefully acidified by the dropwise addition of conc. HCl (92 ml, 1.1 mole). A colorless precipitate formed and this was subsequently collected by filtration. Crystallization from ethanol afforded colorless, chunky crystals, Mp 164°-166° C. was heated to reflux After refluxing overnight the reaction was cooled in an ice bath A colorless precipitate formed this was subsequently collected by filtration Crystallization from ethanol afforded colorless

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

実験手順: A stirred mixture of 1-benzoyl-4-methylthiosemicarbazide (20.9 g, 1.00×10-1 mole) and 1 molar aqueous NaHCO3 (1000 ml, 1 mole) was heated to reflux. After refluxing overnight the reaction was cooled in an ice bath. With stirring the solution was carefully acidified by the dropwise addition of conc. HCl (92 ml, 1.1 mole). A colorless precipitate formed and this was subsequently collected by filtration. Crystallization from ethanol afforded colorless, chunky crystals, Mp 164°-166° C. was heated to reflux After refluxing overnight the reaction was cooled in an ice bath A colorless precipitate formed this was subsequently collected by filtration Crystallization from ethanol afforded colorless

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

実験手順: To a stirred solution of benzoic acid hydrazide (2.35 g, 1.73×10-2 mole) and THF (50 ml) was added a solution of methyl isothiocyanate (1.14 g, 1.56×10-2 mole) and THF (50 ml). The reaction was then refluxed for 2 hours before being cooled. The precipitate was collected by filtration and crystallized from ethanol, affording a colorless solid, Mp 199°-200° C. The reaction was then refluxed for 2 hours before being cooled The precipitate was collected by filtration crystallized from ethanol affording a colorless solid, Mp 199°-200° C.

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

実験手順: To a stirred solution of benzoic acid hydrazide (2.35 g, 1.73×10-2 mole) and THF (50 ml) was added a solution of methyl isothiocyanate (1.14 g, 1.56×10-2 mole) and THF (50 ml). The reaction was then refluxed for 2 hours before being cooled. The precipitate was collected by filtration and crystallized from ethanol, affording a colorless solid, Mp 199°-200° C. The reaction was then refluxed for 2 hours before being cooled The precipitate was collected by filtration crystallized from ethanol affording a colorless solid, Mp 199°-200° C.

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

実験手順: A stirred mixture of 1-benzoyl-4-methylthiosemicarbazide (20.9 g, 1.00×10-1 mole) and 1 molar aqueous NaHCO3 (1000 ml, 1 mole) was heated to reflux. After refluxing overnight the reaction was cooled in an ice bath. With stirring the solution was carefully acidified by the dropwise addition of conc. HCl (92 ml, 1.1 mole). A colorless precipitate formed and this was subsequently collected by filtration. was heated to reflux After refluxing overnight the reaction was cooled in an ice bath A colorless precipitate formed this was subsequently collected by filtration

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

実験手順: A stirred mixture of 1-benzoyl-4-methylthiosemicarbazide (20.9 g, 1.00×10-1 mole) and 1 molar aqueous NaHCO3 (1000 ml, 1 mole) was heated to reflux. After refluxing overnight the reaction was cooled in an ice bath. With stirring the solution was carefully acidified by the dropwise addition of conc. HCl (92 ml, 1.1 mole). A colorless precipitate formed and this was subsequently collected by filtration. was heated to reflux After refluxing overnight the reaction was cooled in an ice bath A colorless precipitate formed this was subsequently collected by filtration

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

実験手順: To a stirred solution of benzoic acid hydrazide (2.35 g, 1.73×10-2 mole) and THF (50 ml) was added a solution of methyl isothiocyanate (1.14 g, 1.56×10-2 mole) and THF (50 ml). The reaction was then refluxed for 2 hours before being cooled. The precipitate was collected by filtration and crystallized from ethanol, affording a colorless solid, Mp 199°-200° C. The reaction was then refluxed for 2 hours before being cooled The precipitate was collected by filtration crystallized from ethanol affording a colorless solid, Mp 199°-200° C.

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

実験手順: A stirred mixture of 1-benzoyl-4-methylthiosemicarbazide (20.9 g, 1.00×10-1 mole) and 1 molar aqueous NaHCO3 (1000 ml, 1 mole) was heated to reflux. After refluxing overnight the reaction was cooled in an ice bath. With stirring the solution was carefully acidified by the dropwise addition of conc. HCl (92 ml, 1.1 mole). A colorless precipitate formed and this was subsequently collected by filtration. Crystallization from ethanol afforded colorless, chunky crystals, Mp 164°-166° C. was heated to reflux After refluxing overnight the reaction was cooled in an ice bath A colorless precipitate formed this was subsequently collected by filtration Crystallization from ethanol afforded colorless

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

実験手順: To a stirred solution of benzoic acid hydrazide (2.35 g, 1.73×10-2 mole) and THF (50 ml) was added a solution of methyl isothiocyanate (1.14 g, 1.56×10-2 mole) and THF (50 ml). The reaction was then refluxed for 2 hours before being cooled. The precipitate was collected by filtration and crystallized from ethanol, affording a colorless solid, Mp 199°-200° C. The reaction was then refluxed for 2 hours before being cooled The precipitate was collected by filtration crystallized from ethanol affording a colorless solid, Mp 199°-200° C.

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

実験手順: A stirred mixture of 1-benzoyl-4-methylthiosemicarbazide (20.9 g, 1.00×10-1 mole) and 1 molar aqueous NaHCO3 (1000 ml, 1 mole) was heated to reflux. After refluxing overnight the reaction was cooled in an ice bath. With stirring the solution was carefully acidified by the dropwise addition of conc. HCl (92 ml, 1.1 mole). A colorless precipitate formed and this was subsequently collected by filtration. Crystallization from ethanol afforded colorless, chunky crystals, Mp 164°-166° C. was heated to reflux After refluxing overnight the reaction was cooled in an ice bath A colorless precipitate formed this was subsequently collected by filtration Crystallization from ethanol afforded colorless

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

実験手順: To a stirred solution of benzoic acid hydrazide (2.35 g, 1.73×10-2 mole) and THF (50 ml) was added a solution of methyl isothiocyanate (1.14 g, 1.56×10-2 mole) and THF (50 ml). The reaction was then refluxed for 2 hours before being cooled. The precipitate was collected by filtration and crystallized from ethanol, affording a colorless solid, Mp 199°-200° C. The reaction was then refluxed for 2 hours before being cooled The precipitate was collected by filtration crystallized from ethanol affording a colorless solid, Mp 199°-200° C.