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3,5 - DibroMo - 2,4 - diMethylpyridine

Product Name
3,5 - DibroMo - 2,4 - diMethylpyridine
CAS No.
29976-20-3
Chemical Name
3,5 - DibroMo - 2,4 - diMethylpyridine
Synonyms
Pyridine, 3,5-dibromo-2,4-dimethyl-;3,5 - DibroMo - 2,4 - diMethylpyridine
CBNumber
CB92583098
Molecular Formula
C7H7Br2N
Formula Weight
264.95
MOL File
29976-20-3.mol
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3,5 - DibroMo - 2,4 - diMethylpyridine Property

Melting point:
32-33 °C
Boiling point:
253.9±35.0 °C(Predicted)
Density 
1.795±0.06 g/cm3(Predicted)
storage temp. 
Sealed in dry,Room Temperature
pka
1.89±0.28(Predicted)
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Hazard and Precautionary Statements (GHS)

Symbol(GHS)
Signal word
Warning
Hazard statements

H302Harmful if swallowed

H315Causes skin irritation

H319Causes serious eye irritation

H335May cause respiratory irritation

Precautionary statements

P261Avoid breathing dust/fume/gas/mist/vapours/spray.

P305+P351+P338IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continuerinsing.

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N-Bromosuccinimide Price

AK Scientific
Product number
3091AB
Product name
3,5-Dibromo-2,4-dimethylpyridine
Packaging
100mg
Price
$145
Updated
2021/12/16
AK Scientific
Product number
3091AB
Product name
3,5-Dibromo-2,4-dimethylpyridine
Packaging
250mg
Price
$201
Updated
2021/12/16
American Custom Chemicals Corporation
Product number
HCH0364197
Product name
3,5-DIBROMO-2,4-DIMETHYLPYRIDINE
Purity
95.00%
Packaging
5MG
Price
$502.08
Updated
2021/12/16
Aaron Chemicals
Product number
AR00BGTS
Product name
3,5-DibroMo-2,4-diMethylpyridine
Purity
98%
Packaging
100mg
Price
$54
Updated
2021/12/16
Aaron Chemicals
Product number
AR00BGTS
Product name
3,5-DibroMo-2,4-diMethylpyridine
Purity
98%
Packaging
250mg
Price
$78
Updated
2021/12/16
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3,5 - DibroMo - 2,4 - diMethylpyridine Chemical Properties,Usage,Production

Synthesis

108-47-4

27063-92-9

29976-20-3

27063-93-0

GENERAL STEPS: Dissolve 2,4-dimethylpyridine (5.39 mL, 46.7 mmol, 1 eq.) in bromide (50 mL) containing 20% free SO3 at 0 °C with stirring. A high efficiency reflux condenser was installed and heated to 165°C in an oil bath. Bromine (4.30 mL, 83.4 mmol, 0.9 eq.) was added in batches over a period of 5 hours, maintaining the temperature at 155-175 °C and stirring for 20 hours. After completion of the reaction, it was cooled to room temperature and the reaction solution was poured into crushed ice (200 g) and stirred for 1 hour. The solution was neutralized with solid Na2CO3 vesicles to an orange solution, diluted with water and extracted with EtOAc (2 x 250 mL). The organic layers were combined, dried with Na2SO4 and concentrated in vacuum. The crude product was purified by automated fast column chromatography (Biotage KP-Sil SNAP 340g column, 0-15% EtOAc/hexane) and dried under vacuum to give three brominated products: 3,5-dibromo-2,4-dimethylpyridine (8), 5-bromo-2,4-dimethylpyridine (9) and 3-bromo-2,4-dimethylpyridine (10). 3,5-Dibromo-2,4-dimethylpyridine (8) is a white solid (1.48 g, 12%) with a melting point of 28-30 °C. 1H NMR (400 MHz, CDCl3) δ 2.54 (s, 3H, CH3), 2.61 (s, 3H, CH3), 8.41 (s, 1H, pyHortho); 13C NMR (100 MHz, CDCl3) δ 23.8 (CH3), 25.7 (CH3), 120.3 (ArC), 124.4 (ArC), 146.4 (ArC), 148.5 (ArCH), 156.5 (ArC); IR νmax (film)/cm?1 3045, 2998, 2956, 2921, 1558, 1433, 1376, 1349, 1232, 1376, 1349, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232, 1232 1376, 1349, 1232, 1049, 993, 928, 783; HRMS (ESI+) m/z calcd for C7H8Br2N [M+H]+ 263.9018, found 263.9027. 5-Bromo-2,4-dimethylpyridine (9) was a colorless oil (1.89 g, 22%).1H NMR (400 MHz, CDCl3) δ 2.32 (s, 3H, CH3), 2.44 (s, 3H, CH3), 7.00 (s, 1H, pyHortho), 8.47 (s, 1H, pyHmeta); 13C NMR ( 100 MHz, CDCl3) δ 22.1 (CH3), 23.6 (CH3), 120.4 (ArC), 125.5 (ArCH), 146.7 (ArC), 150.5 (ArCH), 157.0 (ArC); IR νmax (film)/cm?1 2985, 2957, 2924, 2854, 1592, 1461, 1377 1592, 1461, 1377, 1353, 1289, 1177, 1032; HRMS (ESI+) m/z calcd for C7H9BrN [M+H]+ 185.9913, found 185.9918. 3-Bromo-2,4-dimethylpyridine (10) was a colorless oil (3.04 g, 35%).1H NMR (400 MHz, CDCl3) δ 2.33 (s, 3H, CH3), 2.61 (s, 3H, CH3), 6.91 (d, J = 5.0 Hz, 1H, pyHmeta), 8.18 (d, J = 5.0 Hz, 1H, 2995, 2958, 2922, 1585, 1437, 1389, 1123, 1024, 916, 825; HRMS (ESI+) m/z calcd for C7H9BrN [M+H]+ 185.9913, found 185.9917.

References

[1] Zeitschrift fuer Chemie (Stuttgart, Germany), 1988, vol. 28, # 2, p. 59 - 60
[2] Zeitschrift fuer Chemie (Stuttgart, Germany), 1988, vol. 28, # 2, p. 59 - 60
[3] Patent: WO2010/43866, 2010, A2. Location in patent: Page/Page column 48; 87-88
[4] Organic and Biomolecular Chemistry, 2011, vol. 9, # 1, p. 127 - 135

3,5 - DibroMo - 2,4 - diMethylpyridine Preparation Products And Raw materials

Raw materials

Preparation Products

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3,5 - DibroMo - 2,4 - diMethylpyridine Suppliers

China 26 India 1 United States 2 Global 29
Modachem Shanghai Co., Ltd
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View Lastest Price from 3,5 - DibroMo - 2,4 - diMethylpyridine manufacturers

Career Henan Chemical Co
Product
3,5 - DibroMo - 2,4 - diMethylpyridine 29976-20-3
Price
US $1.00/KG
Min. Order
1KG
Purity
97%-99.9%
Supply Ability
100kg
Release date
2019-12-20

29976-20-3, 3,5 - DibroMo - 2,4 - diMethylpyridineRelated Search:


  • 3,5 - DibroMo - 2,4 - diMethylpyridine
  • Pyridine, 3,5-dibromo-2,4-dimethyl-
  • 29976-20-3