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2,2-DIMETHYL-PIPERAZINE

2,2-DIMETHYL-PIPERAZINE structure

CAS No:
84477-72-5
Formula:
C6H14N2
Chemical Name:
2,2-DIMETHYL-PIPERAZINE
Synonyms:
2,2-Dimethylpiperazine;2,2-DIMETHYL-PIPERAZINE;2,2-Dimethyl piperazine;Piperazine, 2,2-dimethyl-;MFCD06798288;5-dimethylpiperazine;2,2-dimethylpiprazine;2,2-dimethypiperazine;COTARNINECHLORIDE;PubChem17283
Categories:
Pharmaceutical Intermediates > Heterocyclic Compound

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2,2-DIMETHYL-PIPERAZINE Basic Attributes

Molecular Weight：

114.19

Exact Mass：

114.115700

HScode：

2933599090

Characteristics

PSA：

24.1

XLogP3：

-0.2

Density：

0.8±0.1 g/cm3

Flash Point：

38.9±10.2 °C

Refractive Index：

1.417

Safety Information

hazard class code：

42-51/53

safety instructions：

Marks：

Xi,N

Precautionary statement(s)：

P273, P391, P501

Hazard Statements：

H411

2,2-DIMETHYL-PIPERAZINE Use and Manufacturing

A mixture of 3, 3-dimethylpiperazin-2-one (8.28 kg, 64.6 mol) and tetrahydrofuran (THF) (60 kg) is heated to 50-60 °C. giving a slightly unclear solution. THF (50 kg) is stirred under nitrogen, and LIALH4 (250 g, in a soluble plastic bag, from CHEMETALL) is added, which gives a slow evolution of gas. After gas evolution has ceased, more LIALH4 IS added (a total of 3.0 kg, 79.1 mol, is used), and the temperature rises from 22 °C to 50 °C because OF AN EXOTERM. The solution of 3, 3-dimethylpiperazin-2-one is added slowly over 2 hours at 41-59 °C. The suspension is stirred for another hour at 59 °C (jacket temperature 60 °C). The mixture is cooled, and water (3 1) is added over two hours, keeping the temperature below 25 °C (it is necessary to cool with a jacket temperature OF 0 C). Then sodium hydroxide (15percent, 3.50 kg) is added over 20 minutes at 23 °C, cooling necessary. More water (9 1) is added over half an hour (cooling necessary), and the mixture is stirred over night under nitrogen. Filter agent Celit (4 kg) is added, and the mixture is filtered. The filter cake is washed with THF (40 KG). The combined filtrates are concentrated in the reactor until the temperature in the reactor is 70 °C (distillation temperature 66 °C) at 800 mbar. The remanence (12.8 kg) is further concentrated on a rotavapor to approximately 10 1. Finally, the mixture is fractionally distilled at atmospheric pressure, and the product is collected at 163-4 °C. Yield 5.3 kg (72percent). NMR complies with the structure.Synthesis of 2, 2-diniethylpiperazineA mixture of 3, 3-dimethylpiperazin-2-one (8.28 kg, 64.6 mol, large scale preparation analogous to the preparation described in to Example 3) and tetrahydrofuran (THF) (60 kg) is heated to 50-60 Example 4 Synthesis of 2, 2-dimethylpiperazine; A mixture of 3, 3-dimethylpiperazin-2-one (8.28 kg, 64.6 mol, large scale preparation analogous to the preparation described in to Example 3) and tetrahydrofuran (THF) (60 kg) is heated to 50-60 Synthesis of 2, 2-dimethylpiperazineA mixture of 3, 3-dimethylpiperazin-2-one (8.28 kg, 64.6 mol) and tetrahydrofuran (THF) (60 kg) is heated to 50-60

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