Preparation method of piperazine amide compound
A technology of piperazine amides and compounds, which is applied in the field of preparation of piperazine amides, can solve the problems of unfavorable industrial production, high corrosion of equipment, complicated operation, etc., and achieves simple and easy separation and purification, low equipment requirements, and high reaction efficiency. The effect of high yield
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Embodiment 1
[0020] Synthesis of (4-methyl-1-piperazinyl)(1-methyl-1H-2-pyrrolyl)methanone
[0021] Add 14g 1-methylpiperazine hydrochloride, 24g potassium carbonate and 100mL dimethylformamide to a dry round bottom flask, mix well and add 23g 2,2,2-trichloro-1-(1-methyl Base-1H-2-pyrrolyl)ethanone, heated to 100°C and stirred for 10 hours. After the reaction was completed, the dimethylformamide was distilled off under reduced pressure, and the residue was dissolved in 200 mL of ethyl acetate, then washed twice with 200 mL of ammonium chloride aqueous solution, and the ethyl acetate was distilled off under reduced pressure to obtain the target product, with an HPLC purity of 98%. Yield 92%.
Embodiment 2
[0023] Synthesis of (4-methyl-1-piperazinyl)(1-methyl-1H-2-pyrrolyl)methanone
[0024] Add 14g of 1-methylpiperazine hydrochloride, 17g of sodium ethoxide and 100mL of dimethylformamide to a dry round bottom flask, mix well and add 23g of 2,2,2-trichloro-1-(1-methyl Base-1H-2-pyrrolyl)ethanone, stirred at 20°C for 10 hours. After the reaction was completed, water was added to quench, tetrahydrofuran was distilled off under reduced pressure, and the residue was dissolved with 200 mL of ethyl acetate, then washed twice with 200 mL of aqueous ammonium chloride solution, and ethyl acetate was distilled off under reduced pressure to obtain the target product, with an HPLC purity of 98%. Yield 80%.
Embodiment 3
[0026] tert-butyl 4-(1-methyl-1H-pyrrolyl-2-carbonyl)piperazine-1-carboxylate
[0027] Add 22g of 1-tert-butoxycarbonylpiperazine, 35g of potassium carbonate and 100mL of dimethylformamide to a dry round bottom flask, mix well and add 21g of 2,2,2-trichloro-1-(1-methyl -1H-2-pyrrolyl)ethanone, heated to 70°C and stirred for 10 hours. After the reaction was completed, the dimethylformamide was distilled off under reduced pressure, and the residue was dissolved in 200 mL of ethyl acetate, then washed twice with 200 mL of ammonium chloride aqueous solution, and the ethyl acetate was distilled off under reduced pressure to obtain the target product, with an HPLC purity of 98%. Yield 85%.
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