Identification | Back Directory | [Name]
4-bromo-1-tert-butyl-1H-pyrazole | [CAS]
70951-85-8 | [Synonyms]
4-Bromo-1-t-butylpyrazole 1-tert-Butyl-4-Bromopyrazole 4-Bromo-1-tert-butylpyrazole 4-bromo-1-t-butyl-1H-pyrazole 4-bromo-1-tert-butyl-1H-pyrazole 1H-Pyrazole, 4-bromo-1-(1,1-dimethylethyl)- | [Molecular Formula]
C7H11BrN2 | [MDL Number]
MFCD13195703 | [MOL File]
70951-85-8.mol | [Molecular Weight]
203.08 |
Chemical Properties | Back Directory | [Boiling point ]
229.8±13.0℃ (760 Torr) | [density ]
1.37±0.1 g/cm3 (20 ºC 760 Torr) | [Fp ]
92.8±19.8℃ | [storage temp. ]
Sealed in dry,2-8°C | [Appearance]
Colorless to light yellow Liquid | [InChI]
InChI=1S/C7H11BrN2/c1-7(2,3)10-5-6(8)4-9-10/h4-5H,1-3H3 | [InChIKey]
KLLXOOSSATXFFY-UHFFFAOYSA-N | [SMILES]
N1(C(C)(C)C)C=C(Br)C=N1 |
Hazard Information | Back Directory | [Synthesis]
1. N-bromosuccinimide (NBS, 2.63 kg, 14.79 mol) was added batchwise to a solution of 1-tert-butylpyrazole (1.75 kg, 14.09 mol) in dichloromethane (12.9 kg) in an ice bath at 0°C to 10°C. The reaction was carried out by gas chromatography (GC).
2. The reaction mixture was kept stirred at 0 °C until the content of 1-tert-butylpyrazole was below 30% as shown by gas chromatography (GC) analysis.
3. the reaction mixture was gradually warmed to room temperature with continued stirring until the GC analysis showed that the content of 1-tert-butylpyrazole was less than 1.0%.
4. Upon completion of the reaction, 10% aqueous sodium bisulfite was added to the reaction mixture until it no longer showed blue color when detected using KI-starch test paper.
5. The organic phase was washed sequentially with 5% sodium chloride solution and saturated brine.
6. Evaporate the organic phase under pressure to obtain 4-bromo-1-tert-butyl-1H-pyrazole as a brown liquid (2.67 kg, yield 93.4%; GC purity 99.1%). | [References]
[1] Patent: WO2011/134971, 2011, A1. Location in patent: Page/Page column 16; 17; 72 [2] Patent: WO2008/33999, 2008, A2. Location in patent: Page/Page column 84 [3] Patent: WO2014/1377, 2014, A1. Location in patent: Page/Page column 104 [4] Patent: US2013/40984, 2013, A1. Location in patent: Paragraph 0393-0395 [5] Patent: WO2017/42100, 2017, A1. Location in patent: Page/Page column 43 |
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Company Name: |
Energy Chemical
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Tel: |
021-021-58432009 400-005-6266 |
Website: |
http://www.energy-chemical.com |
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