(4-chloroanilino)thiourea

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Twelve g of 1-(4-chlorophenyl)thiosemicarbazide was suspended in 60 ml of 95% formic acid, and the mixture was stirred under reflux for 24 hours. The mixture was then cooled, and the product precipitated. It was collected and washed with cold denatured ethanol, and was dried to obtain 6.1 g of the desired intermediate, m.p. 222°-224°. under reflux for 24 hours The mixture was then cooled the product precipitated It was collected washed was dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Fifty g of 4-chlorophenylhydrazine hydrochloride and 40 g of ammonium thiocyanate were added to 250 ml of denatured ethanol and the mixture was stirred under reflux for 16 hours. It was then filtered while still hot and the filter cake was washed with about 100 ml of hot ethanol. As the filtrate cooled, the product began to crystallize, and it was collected and recrystallized from denatured ethanol to obtain 32.7 g of the desired intermediate, m.p. 200°-201°. under reflux for 16 hours It was then filtered while still hot and the filter cake was washed with about 100 ml of hot ethanol As the filtrate cooled to crystallize it was collected recrystallized from denatured ethanol