4,5-dibroMo-3-nitro-1H-pyrazole
- Product Name
- 4,5-dibroMo-3-nitro-1H-pyrazole
- CAS No.
- 104599-37-3
- Chemical Name
- 4,5-dibroMo-3-nitro-1H-pyrazole
- Synonyms
- 100083;3,4-DibroMo-5-nitro-1H-pyrazole;4,5-dibroMo-3-nitro-1H-pyrazole;1H-Pyrazole, 3,4-dibromo-5-nitro-
- CBNumber
- CB32552717
- Molecular Formula
- C3HBr2N3O2
- Formula Weight
- 270.87
- MOL File
- 104599-37-3.mol
4,5-dibroMo-3-nitro-1H-pyrazole Property
- Boiling point:
- 365.6±37.0 °C(Predicted)
- Density
- 2.419
- storage temp.
- under inert gas (nitrogen or Argon) at 2-8°C
- pka
- 3.91±0.50(Predicted)
- Appearance
- Off-white to light yellow Solid
Hazard and Precautionary Statements (GHS)
- Symbol(GHS)
-
- Signal word
- Warning
- Hazard statements
-
H315Causes skin irritation
H319Causes serious eye irritation
H335May cause respiratory irritation
- Precautionary statements
-
P261Avoid breathing dust/fume/gas/mist/vapours/spray.
P264Wash hands thoroughly after handling.
P264Wash skin thouroughly after handling.
P271Use only outdoors or in a well-ventilated area.
P280Wear protective gloves/protective clothing/eye protection/face protection.
P302+P352IF ON SKIN: wash with plenty of soap and water.
P304+P340IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
P305+P351+P338IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continuerinsing.
P312Call a POISON CENTER or doctor/physician if you feel unwell.
P321Specific treatment (see … on this label).
P332+P313IF SKIN irritation occurs: Get medical advice/attention.
P337+P313IF eye irritation persists: Get medical advice/attention.
P362Take off contaminated clothing and wash before reuse.
P403+P233Store in a well-ventilated place. Keep container tightly closed.
P405Store locked up.
P501Dispose of contents/container to..…
N-Bromosuccinimide Price
- Product number
- P000649286
- Product name
- 3,4-Dibromo-5-nitro-1H-pyrazole
- Purity
- 95+%
- Packaging
- 100mg
- Price
- $20
- Updated
- 2021/12/16
- Product number
- P000649286
- Product name
- 3,4-Dibromo-5-nitro-1H-pyrazole
- Purity
- 95+%
- Packaging
- 250mg
- Price
- $31
- Updated
- 2021/12/16
- Product number
- P000649286
- Product name
- 3,4-Dibromo-5-nitro-1H-pyrazole
- Purity
- 95+%
- Packaging
- 1g
- Price
- $77
- Updated
- 2021/12/16
- Product number
- HCH0364116
- Product name
- 3,4-DIBROMO-5-NITRO-1H-PYRAZOLE
- Purity
- 95.00%
- Packaging
- 5MG
- Price
- $501.46
- Updated
- 2021/12/16
- Product number
- 1026AA
- Product name
- 3,4-Dibromo-5-nitro-1H-pyrazole
- Packaging
- 5g
- Price
- $2080
- Updated
- 2021/12/16
4,5-dibroMo-3-nitro-1H-pyrazole Chemical Properties,Usage,Production
Synthesis
67-51-6
17635-44-8
104599-37-3
To a solution of 3,4,5-tribromopyrazole (60 g) in acetic acid (900 mL) was slowly added 90% fuming nitric acid (21 mL) at 10 °C. Subsequently, acetic anhydride (300 mL) was added dropwise over 20 minutes. The reaction system was gradually warmed to room temperature and stirred continuously for 3 hours. Upon completion of the reaction, the mixture was poured onto ice and a white solid precipitated. The precipitate was collected by filtration and washed with water (200 mL). The resulting solid was dissolved in toluene (750 mL), the organic phase was washed sequentially with water (200 mL) and saturated saline (100 mL), dried over anhydrous sodium sulfate and filtered. To this toluene solution was added 3,5-dimethyl-1H-pyrazole (20 g) and heated to reflux for 20 min. The reaction solution was cooled and concentrated under reduced pressure. The crude product was ground with heptane, the precipitate was collected by filtration and dried under vacuum to give a crude product containing mainly the target product (71.7 g, 67.6% yield), which could be used directly in the next reaction. The reduction reaction was carried out by refluxing 3,4-dibromo-5-nitro-1H-pyrazole (69 g) prepared above with stannous chloride dihydrate (135 g) in a mixed solvent of ethyl acetate (600 mL) and ethanol (300 mL) at 110 °C for 45 min. After the reaction was completed, the yellow homogeneous solution was cooled to room temperature and slowly poured into a vigorously stirred mixture of aqueous sodium bicarbonate (33 g) (200 mL) and ethyl acetate (800 mL). Diatomaceous earth (30 g) was added to aid filtration, filtered, and the filter cake was washed with ethyl acetate (600 mL). The organic phases were combined, washed with saturated saline (200 mL), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give an orange oily crude product. Purification by fast column chromatography (Biotage, Quad 25; eluent: dichloromethane solution of 6% ethanol) gave the title compound as a light beige solid (13.2 g, 32% yield). 1H NMR (400 MHz, DMSO-d6) δ: 5.20 (m, 3H), 11.60 (br s, 1H).
References
[1] Patent: US2013/324547, 2013, A1. Location in patent: Paragraph 0520
4,5-dibroMo-3-nitro-1H-pyrazole Preparation Products And Raw materials
Raw materials
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