4-甲基-1-哌嗪-1-基戊烷-1-one

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: By the method of Example I, 2.00 g 2-chloro-5,6-dimethoxy benzimidazole and 4.00 g N-(4-methyl valeroyl) piperazine were reacted in 15 ml. 2-methoxy ethanol to give the desired product as a base; which was converted to the hydrochloride with HCl in isopropyl alcohol. Yield: 3.31 g (89%) mp 255°-257° C.

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

实验步骤: By the method of Example I, 2.00 g 2-chloro-5,6-dimethoxy benzimidazole and 4.00 g N-(4-methyl valeroyl) piperazine were reacted in 15 ml. 2-methoxy ethanol to give the desired product as a base; which was converted to the hydrochloride with HCl in isopropyl alcohol. Yield: 3.31 g (89%) mp 255°-257° C.

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

实验步骤: 60 g 4-methylvaleric acid was converted to the acid chloride by heating 1 hour with 120 g thionyl chloride. Distillation gave 45.2 g (65%) 4-methyl valeroyl chloride, bp 35°-38° C/10.0 mm. This product in 100 ml benzene was added to a solution of 56 g N-benzyl piperazine and 33.8 g triethylamine in 250 ml benzene. After 1 hour at 25° a solution of 47 g potassium carbonate in 250 ml water was added. The benzene layer was removed and concentrated. The crude N-(4-methyl valeroyl) N'-benzyl piperazine was hydrogenated in 300 ml ethanol using 16 g 5% pd/catalyst. The product was distilled to give 40.2 g product, bp 110°-115° C/0.1 mm. (65%) The benzene layer was removed concentrated The product was distilled

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

实验步骤: By the method of Example I, 2.00 g 2-chloro-5,6-dimethoxy benzimidazole and 4.00 g N-(4-methyl valeroyl) piperazine were reacted in 15 ml. 2-methoxy ethanol to give the desired product as a base; which was converted to the hydrochloride with HCl in isopropyl alcohol. Yield: 3.31 g (89%) mp 255°-257° C.

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

实验步骤: 60 g 4-methylvaleric acid was converted to the acid chloride by heating 1 hour with 120 g thionyl chloride. Distillation gave 45.2 g (65%) 4-methyl valeroyl chloride, bp 35°-38° C/10.0 mm. This product in 100 ml benzene was added to a solution of 56 g N-benzyl piperazine and 33.8 g triethylamine in 250 ml benzene. After 1 hour at 25° a solution of 47 g potassium carbonate in 250 ml water was added. The benzene layer was removed and concentrated. The crude N-(4-methyl valeroyl) N'-benzyl piperazine was hydrogenated in 300 ml ethanol using 16 g 5% pd/catalyst. The product was distilled to give 40.2 g product, bp 110°-115° C/0.1 mm. (65%) The benzene layer was removed concentrated The product was distilled