ChemicalBook CAS DataBase List 1-Methylpiperazine

1-Methylpiperazine synthesis

15synthesis methods

Product Name:1-Methylpiperazine
CAS Number:109-01-3
Molecular formula:C5H12N2
Molecular Weight:100.16

16339-07-4
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109-01-3
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6928-85-4 Synthesis

6928-85-4
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$9.00/5g

Yield:6928-85-4 96%

Reaction Conditions:

with carbon dioxide;water;ammonium chloride;zinc at 35; under 1500.15 Torr; for 1.5 h;Autoclave;Green chemistry;Reagent/catalyst;Temperature;Pressure;

Steps:

Synthesis of N-amino aza-aliphatic cyclic compounds 2a-c, 5a,b, 7a,b, and 9

General procedure: A solution ofN-nitroso aza-aliphatic cyclic compound 1a-c, 4a,b, 6a,b, or 8 (1.0 mol) in H2O (250 ml) was placed into a 1-l autoclave equipped with a CO2 ventilation device, a gas flow meter, and a barometer. NH4Cl (5.35 g, 0.1 mol) was added to the solution and the system was charged with CO2 at a flow rate 30 l/h. After stirring for 20 min, the mixture was heated to 35°C and zinc powder (163 g, 2.5 mol) was added in portions (16.3 g every 6 min). The pressure in the closed system was maintained at 0.2 MPa and temperature at 35°C. After addition of all zinc (about 1 h), the reaction mixture was stirred at 35°C for 0.5 h and then analyzed by GC. The resulting ZnCO3 was filtered off and washed with H2O (150 ml). The filtrate was transferred to a 1-l three neck round-bottom flask, H2O was removed under reduced pressure, and vacuum distillation at 60-135 °C (internal temperature) was performed to afford products 2a-c, 5a,b, 7a,b, and 9. 4-Methylpiperazin-1-amine (2a).15 Yield 110 g (96%),colorless liquid, bp 75-80°C (30-40 mmHg). 1H NMR spectrum, δ, ppm: 3.11 (2H, s, NH2); 2.94-2.30 (8H, m,CH2); 2.25 (3H, s, CH3). Mass spectrum, m/z (Irel, %): 115[M]+ (100).

References:

Yang, Weiqing;Lu, Xiang;Zhou, Tingting;Cao, Yongjing;Zhang, Yuanyuan;Ma, Menglin [Chemistry of Heterocyclic Compounds,2018,vol. 54,# 8,p. 780 - 783][Khim. Geterotsikl. Soedin.,2018,vol. 54,# 8,p. 780 - 783,4]