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3-FLUORO-5-METHYLBENZOIC ACID

Product Name
3-FLUORO-5-METHYLBENZOIC ACID
CAS No.
518070-19-4
Chemical Name
3-FLUORO-5-METHYLBENZOIC ACID
Synonyms
RARECHEM AL BO 2238;3-Fluoro-5-methybenzoic acid;3-FLUORO-5-METHYLBENZOIC ACID;3-Fluoro-5-methylbenzoicacid98%;Benzoic acid, 3-fluoro-5-methyl-;Benzoic acid, 3-fluoro-5-methyl- (9CI);3-Carboxy-5-fluorotoluene, 5-Fluoro-m-toluic acid
CBNumber
CB7666038
Molecular Formula
C8H7FO2
Formula Weight
154.14
MOL File
518070-19-4.mol
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3-FLUORO-5-METHYLBENZOIC ACID Property

Melting point:
141-143℃
Boiling point:
266.2±20.0 °C(Predicted)
Density 
1.258±0.06 g/cm3(Predicted)
storage temp. 
Sealed in dry,Room Temperature
form 
powder
pka
3.93±0.10(Predicted)
color 
White
Water Solubility 
Soluble in water (25°C)
InChI
InChI=1S/C8H7FO2/c1-5-2-6(8(10)11)4-7(9)3-5/h2-4H,1H3,(H,10,11)
InChIKey
XPUFVYIUPYNLPD-UHFFFAOYSA-N
SMILES
C(O)(=O)C1=CC(C)=CC(F)=C1
CAS DataBase Reference
518070-19-4(CAS DataBase Reference)
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Safety

Hazard Codes 
Xi
HazardClass 
IRRITANT
HS Code 
2916310090
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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.

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.

P405Store locked up.

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N-Bromosuccinimide Price

TRC
Product number
F593175
Product name
3-Fluoro-5-methylbenzoicAcid
Packaging
50g
Price
$290
Updated
2021/12/16
TRC
Product number
F593175
Product name
3-Fluoro-5-methylbenzoicAcid
Packaging
1g
Price
$65
Updated
2021/12/16
TRC
Product number
F593175
Product name
3-Fluoro-5-methylbenzoicAcid
Packaging
10g
Price
$105
Updated
2021/12/16
SynQuest Laboratories
Product number
2721-3-X7
Product name
3-Fluoro-5-methylbenzoic acid
Purity
98%
Packaging
25g
Price
$106
Updated
2021/12/16
Matrix Scientific
Product number
009530
Product name
3-Fluoro-5-methylbenzoic acid
Purity
98%
Packaging
25g
Price
$107
Updated
2021/12/16
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3-FLUORO-5-METHYLBENZOIC ACID Chemical Properties,Usage,Production

Chemical Properties

off white powder

Uses

3-Fluoro-5-methylbenzoic Acid is an intermediate used to prepare five-membered heterocyclic compound as mGluR5 receptor antagonists.

Synthesis

660416-38-6

518070-19-4

1. 30 mL of concentrated hydrochloric acid was slowly added to 75 mL of an aqueous suspension containing 20 g (95.6 mmol) of dimethyl 5-aminoisophthalate at -5 °C. Subsequently 7.5 g (109 mmol) of sodium nitrite was added in batches and the reaction mixture was stirred for 15 minutes. 2. 18 mL (100 mmol, 48% aqueous solution) of tetrafluoroboric acid was added and the mixture continued to be stirred for 30 minutes at 0 °C. The reaction mixture was purified by filtration. The precipitate was collected by filtration and washed with 60 mL of cold methanol and 60 mL of ether. 3. The residue was heated to decomposition in an oil bath at about 110°C. After cooling, it was diluted with ether, concentrated and purified by rapid chromatography on silica gel using 5% ethyl acetate/hexane as eluent to give 9.0 g (44%) of white fluffy solid product. 4. A 41 mL methanol suspension of 1.7 g (8.0 mmol) dimethyl 5-fluoroisophthalate was mixed with 7.2 mL (7.2 mmol) of 1.0 N sodium hydroxide and stirred overnight at room temperature. After concentration, the residue was dissolved in water, transferred to a partition funnel, and the aqueous layer was washed three times with dichloromethane, followed by acidification to pH 2 with 1.0 N hydrochloric acid. 5. The precipitate was extracted with ethyl acetate, washed with brine and dried over anhydrous sodium sulfate. The solvent was removed in vacuum to give 1.3 g (83%) of 5-fluoroisophthalic acid monomethyl ester as a white solid. 6. In an ice bath, 2.2 mL (16.0 mmol) of triethylamine and 1.0 mL (8.0 mmol) of isobutyl chloroformate were added to a 20 mL solution of dichloromethane with 1.3 g (6.7 mmol) of mono-methyl 5-fluoroisophthalate, which was subsequently warmed to room temperature and stirred for 2 hours. After filtration and concentration, the residue was dissolved in 10 mL of tetrahydrofuran and 3 mL of a 3 mL aqueous solution of 1.1 g (29.02 mmol) of sodium borohydride was slowly added. 7. After 1 hour of reaction, it was quenched with methanol, diluted with ethyl acetate, washed with water and brine, dried over anhydrous sodium sulfate, filtered and concentrated. Purification by rapid column chromatography on silica gel using 30% ethyl acetate/hexane as eluent gave 667 mg (54%) of methyl 3-fluoro-5-hydroxymethylbenzoate as a colorless oil. 8. 2 mL of ethanol was added to a round-bottomed flask containing 667 mg (3.6 mmol) methyl 3-fluoro-5-hydroxymethylbenzoate and 300 mg 10% palladium/activated carbon under argon protection. The flask was evacuated and filled with hydrogen and stirred for 2 h. The catalyst was removed by filtration through diatomaceous earth and the filtrate was concentrated to give 520 mg (87%) of methyl 3-fluoro-5-methylbenzoate. 9. 7.4 mL (3.7 mmol) of 0.5 N lithium hydroxide was added to a 7.4 mL solution of methyl 3-fluoro-5-methylbenzoate in tetrahydrofuran at 75 °C and stirred for 2 hours. After the solvent was removed in vacuum, the residue was dissolved in a small amount of water and acidified to pH 2 with 10% aqueous hydrochloric acid. 10. After extraction with ethyl acetate, the organic layer was washed with water and saturated brine, dried over anhydrous sodium sulfate, filtered and concentrated to give 469 mg (98%) 3-fluoro-5-methylbenzoic acid as a white solid.

References

[1] Patent: WO2004/14881, 2004, A2. Location in patent: Page 100-101

3-FLUORO-5-METHYLBENZOIC ACID Preparation Products And Raw materials

Raw materials

Preparation Products

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3-FLUORO-5-METHYLBENZOIC ACID Suppliers

Shanghai Harvest Chemical Industrial Co., Ltd.
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View Lastest Price from 3-FLUORO-5-METHYLBENZOIC ACID manufacturers

Career Henan Chemical Co
Product
3-FLUORO-5-METHYLBENZOIC ACID 518070-19-4
Price
US $3.00/KG
Min. Order
1KG
Purity
98%
Supply Ability
200KG
Release date
2020-01-12