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Type | HazMat fee for 500 gram (Estimated) |
Excepted Quantity | USD 0.00 |
Limited Quantity | USD 15-60 |
Inaccessible (Haz class 6.1), Domestic | USD 80+ |
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CAS No. : | 396133-32-7 | MDL No. : | MFCD09971266 |
Formula : | C7H16N2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 128.22 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Danger | Class: | 3 |
Precautionary Statements: | P210-P261-P280-P303+P361+P353-P305+P351+P338-P370+P378-P403+P235-P405-P501 | UN#: | 1993 |
Hazard Statements: | H226-H302-H315-H319-H335 | Packing Group: | Ⅲ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A solution of lithium aluminium hydride in tetrahydrofuran (THF) (1.0 M, Aldrich cat. no. 21,277-6, 90 ml) is heated to 50 C on an oil batch. Crude 3,3, 4-trimethylpiperazin-2-one (10 g) is suspended in THF and is slowly added, giving evolution of gas. The resulting mixture is stirred at 45-56 C for 4 hours, giving full conversion to the title compound according to NMR (no signal at 1.2 ppm from starting material). The mixture is cooled, and water (3.3 ml) is added, giving evolution of gas. Then a solution of sodium hydroxide in water (15%, 3.3 ml) is added, giving more gas, and finally water (10 ml) is added. The mixture is filtered, and the filter cake is washed with THF (100 ml). The filtrates are concentrated on a rotary evaporator (0.3 atm. and 60 C in the water batch). The residue is dissolved in THF (200 ml) and dried with sodium sulphate, then the mixture is filtered, and the filtrate is concentrated on a rotary evaporator (0.2 atm and 60 C in the water batch) giving 6.4 grams of the title compound. NMR complies with the structure, the substance contains some THF. | ||
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0℃; for 4.5h;Reflux; | a solution of 3,3,4- trimethylpiperazin-2-one (0.83 g, 5.84 mmol) in tetrahydrofuran (THF; 25 mL) was added lithium aluminum hydride (LAH) (0.17 g, 4.47 mmol) portion- wise at 0 C, and the reaction mixture was heated at reflux for 4.5 h. The reaction mixture was quenched with cold aq. NH4C1 (20 mL) and extracted with DCM (3 x 25 mL). The organic layer was separated, dried over anhydrous Na2S04 and concentrated in vacuo. The crude obtained was purified by triturating with pentane (10 mL) and Et20 (3 mL) to afford 1,2,2-trimethylpiperazine (0.31 g crude) as a grey solid. LC/MS (ESI) m/e [M+H]+/RT (min)/%: 129.00/2.50/86.5%. 1H NMR (400 MHz, DMSO- e) delta 0.90 (s, 6H), 1.55 (s, 1H), 2.02 (s, 3H), 2.21-2.29 (m, 2H), 2.35 (s, 2H), 2.60-2.66 (m, 2H). | |
LiAIH4 (1 M in THF, 47 mL, 47 mmol, 1.5 equiv) was added to a solution of 3,3,4-trimethyl- piperazin-2-one (Step 107.3) (4.5 g, 32 mmol) in THF (50 mL) at 500C, under an argon atmosphere. The resulting mixture was stirred for 2 h at 500C, quenched by addition of acetone, filtered through a pad of celite and concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 94:5:1 ) to afford 1.9 g of the title compound as a yellow oil. Title compound: ESI-MS: 129.1 [M+H]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate; In toluene; at 20 - 45℃; for 2h; | To a suspension of K2CO3 (566 mg, 4.09 mmol, 0.525 equiv.) in toluene (20 mL) was added 1,2,2-trimethyl-piperazine (1.00 g, 7.8 mmol), followed by dropwise addition of a solution of 1 -bromo-2,4-difluoro-5 -nitrobenzene (0.98 mL, 7.8 mmol) in toluene (3 mL) over 2 min. The resulting mixture was stirred at rt for 30 min, then 45 C for 1.5 h resulting in an abundance of yellow precipitate. After diluting with H20 (20 mL) to dissolve the insoluble salts, it was extracted with EtOAc (20 mL x 2). The combined extracts were concentrated and dried under vacuum to give the nitro intermediate as an orange red oil. LCMS [M + H]+ 346.2. To a solution of the above orange oil in MeOH (30 mL) was added a suspension of Raney-Nickel (334 mg, 3.9 mmol) in MeOH (5 mL), followed by hydrazine monohydrate (1.14 mL, 23.4 mmol) dropwise over 2 min. After addition, the reaction mixture was stirred at rt for 30 min. Additional Raney-Nickel (334 mg, 3.9 mmol) in MeOH (5 mL) and hydrazine monohydrate (1.14 mL, 23.4 mmol) were added, followed by THF (15 mL) to make a clear solution. The resulting mixture was heated at 60 C for 30 min. Additional THF (10 mL) and hydrazine monohydrate (0.38 mL, 7.8 mmol) were added and it was heated at 60 C for 30 min. After filtration, the filtrate was concentrated to give a dark brown liquid which was purified by flash chromatography (gradient: EtO Ac/hex 0-100% then MeOH/DCM 0-10%) to give the title compound as a beige solid (1.796 g, 68%). LCMS [M + H]+ 316.2. |