piperazine-1-carbothioamide

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

Procedure: By using the process described in Example 1, but replacing 4-methyl-1-piperazinyl-thiocarboxamide by an equivalent amount of 1-piperazinyl-thiocarboxamide, 2-piperazinyl-4-tert.buty-thiazole dihydrochloride, having a M.P. of 190°-196°, is obtained. The free base is obtained therefrom by treatment with an aqueous sodium hydroxide solution. is obtained The free base is obtained

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

Procedure: Prepared in analogy to example 49 (a) from 1-piperazinecarbothioamide and 1-bromo-4,4,4-trifluoro-butan-2-one. The crude material was purified by chromatography (SiO2, methanol/dichloromethane) to yield the title compound as a brown oil (yield 24%). MS (m/e): 252.3 (M+H+, 100%). The crude material was purified by chromatography (SiO2, methanol/dichloromethane)

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

Procedure: Prepared in analogy to example 49 (a) from 1-piperazinecarbothioamide and 3-bromo-1,1,1-trifluoro-2-butanone. The crude material was purified by chromatography (SiO2, methanol/dichloromethane) to yield the title compound as a white crystalline solid (yield 25%). MS (m/e): 252.1 (M+H+, 100%). The crude material was purified by chromatography (SiO2, methanol/dichloromethane)

Conditions: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a solution of 6.89 mmol 1-piperazinecarbothioamide in 10 ml ethanol was added 8.26 mmol 3-bromo-1,1,1-trifluoroacetone and the mixture was heated at 70° C. for 2 h. The mixture was then concentrated in vacuo and the residue resuspended in dichloromethane. Insoluble material was removed by filtration and the filtrate was concentrated in vacuo. Chromatography (SiO2, methanol/dichloromethane) afforded the title compound as a yellow crystalline solid (yield 41%). MS (m/e): 238.1 (M+H+, 100%). The mixture was then concentrated in vacuo Insoluble material was removed by filtration the filtrate was concentrated in vacuo

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

Procedure: By using the process described in Example 1, but replacing 4-methyl-1-piperazinyl-thiocarboxamide by an equivalent amount of 1-piperazinyl-thiocarboxamide, 2-piperazinyl-4-tert.buty-thiazole dihydrochloride, having a M.P. of 190°-196°, is obtained. The free base is obtained therefrom by treatment with an aqueous sodium hydroxide solution. is obtained The free base is obtained