Overview Synthesis method The effect of nitric acid concentration, reaction temperature and reaction time on the synthesis of products Application
ChemicalBook > CAS DataBase List > Methyl 4-tert-butylbenzoate

Methyl 4-tert-butylbenzoate

Overview Synthesis method The effect of nitric acid concentration, reaction temperature and reaction time on the synthesis of products Application
Product Name
Methyl 4-tert-butylbenzoate
CAS No.
26537-19-9
Chemical Name
Methyl 4-tert-butylbenzoate
Synonyms
RARECHEM AL BF 0269;TIMTEC-BB SBB000305;METHYL 4-T-BUTYLBENZOATE;Methyl 4-tert-butylbenzoat;Methyl p-tert-butylbenzoate;butylbenzoicacidmethylester;METHYL 4-TERT-BUTYLBENZOATE;Methyl 4-Tert-Buthylbenzoate;Methyl4-tert-Butylbenzoate>4-tert-Butylbenzoic acid methyl
CBNumber
CB5134874
Molecular Formula
C12H16O2
Formula Weight
192.25
MOL File
26537-19-9.mol
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Methyl 4-tert-butylbenzoate Property

Boiling point:
122-124 °C9 mm Hg(lit.)
Density 
0.995 g/mL at 25 °C(lit.)
vapor pressure 
1.36hPa at 20℃
refractive index 
n20/D 1.51(lit.)
Flash point:
>230 °F
storage temp. 
Sealed in dry,Room Temperature
form 
Liquid
Specific Gravity
0.995
color 
Clear colorless to yellow
Water Solubility 
35mg/L at 20℃
InChIKey
UPIJOAFHOIWPLT-UHFFFAOYSA-N
LogP
4.3 at 25℃
CAS DataBase Reference
26537-19-9(CAS DataBase Reference)
NIST Chemistry Reference
4-Tert-butylbenzoic acid methyl ester(26537-19-9)
EPA Substance Registry System
Benzoic acid, 4-(1,1-dimethylethyl)-, methyl ester (26537-19-9)
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Safety

Safety Statements 
24/25
WGK Germany 
3
TSCA 
Yes
HS Code 
29163990
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Hazard and Precautionary Statements (GHS)

Symbol(GHS)
Signal word
Warning
Precautionary statements

P280Wear protective gloves/protective clothing/eye protection/face protection.

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N-Bromosuccinimide Price

Sigma-Aldrich
Product number
167533
Product name
Methyl 4-tert-butylbenzoate
Purity
99%
Packaging
25g
Price
$192
Updated
2023/06/20
TCI Chemical
Product number
M1693
Product name
Methyl 4-tert-Butylbenzoate
Purity
>98.0%(GC)
Packaging
25g
Price
$17
Updated
2024/03/01
TCI Chemical
Product number
M1693
Product name
Methyl 4-tert-Butylbenzoate
Purity
>98.0%(GC)
Packaging
500g
Price
$115
Updated
2024/03/01
Alfa Aesar
Product number
A18619
Product name
Methyl 4-tert-butylbenzoate, 98+%
Packaging
25g
Price
$23.65
Updated
2024/03/01
Alfa Aesar
Product number
A18619
Product name
Methyl 4-tert-butylbenzoate, 98+%
Packaging
100g
Price
$32.65
Updated
2024/03/01
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Methyl 4-tert-butylbenzoate Chemical Properties,Usage,Production

Overview

Methyl 4-tert-butylbenzoate appears as white crystalline powder, being slightly soluble in water with the water solubility of 0.006g/100ml Water at 20 ° C. It can be miscible in ethanol, ether and other organic solvents with the organic toluene solubility of 9.0%, being an important organic synthesis intermediates. It is an important additive during the production of PVC heat stabilizer, PP nucleating agent, sunscreen and scaling powder. As the alkyd resin modifier, it can improve the resin luster, color, and speed up the resin drying time and improve the chemical resistance of the performance. The ammonium salt can improve the performance of friction parts and prevent rust, thus can be used as the additives of cutting oil and lubricants. Its sodium salt, barium salt, zinc salt can be used as polymer stabilizer and nucleating agent.

Synthesis method

The synthesis method of P-tert-butyl benzoic acid includes:
The oxidation method of liquid phase solvent, take acetic acid as solvent, lead acetate as oxidant and synthesize p-tert-butyl benzoic acid at low temperature.
Liquid non-solvent oxidation method: there is no need of any solvent; take cobalt acetate and sodium bromide as a catalyst and apply air oxidation at 170e temperature to obtain the final products.
High temperature gas phase oxidation method, in the presence of catalyst, high temperature lead to vaporization and oxidation of p-tert-butyl toluene to generate p-tert-butyl benzoic acid.
Recently, we found that there is no need of any catalyst if using cheap nitric acid as the oxidant for oxidation of p-tert-butyl toluene to get the crude t-butyl benzoic acid, followed by being dissolved with sodium hydroxide to remove organic impurities and insoluble matter, and then being acidified to obtain pure p-tert-butyl benzoic acid. This method has good selectivity and low energy consumption, and can avoid the shortcomings of air oxidation method such as low oxidation conversion rate, thus having great practical value.
Preparation of crude p-tert-butyl benzoic acid:
To a 500 mL autoclave, add 26 mL (0.2 mol, 29.6 g) of p-tert-butyltoluene, 26 mL 68% nitric acid (0.4 mol, 37 g) and 2.5 mL of water. The reaction stirrer was started and the temperature was raised to 180e. The reaction lasted for 8 hour followed by cooling with cool water. Open the reactor with most of the solid being deposited on the bottom of the reactor and attached to the reactor cooling tube in a small amount. The solid was collected, filtered and dried to give 34.5 g with a yield of 95.5%.
The purification of P-tert-butylbenzoic acid
Weigh 10 g of sodium hydroxide and add 90 mL of water to prepare a 10% sodium hydroxide solution. Add the above solid into it. After being sufficiently dissolved, the filtrate was adjusted to pH 3 with hydrochloric acid, and a large amount of crystals would be precipitated at this time. The solution was allowed to stand for 33.4 g with a yield of 98.2%. The product was analyzed by infrared spectroscopy, displaying the characteristic peaks of p-tert-butylbenzoic acid. The content was 98.4% by HPLC analysis with a melting point of 164~166e (literature values 164~165e).

The effect of nitric acid concentration, reaction temperature and reaction time on the synthesis of products

  • Effect of nitric acid concentration on the product
A series of nitric acid concentration experiments were carried out at two temperatures. The reaction temperature of curve 1 was 160e and the reaction temperature of curve 2 was 180e. The product content was obtained by liquid chromatography (HPLC) normalization. It can be seen that with the decrease of nitric acid concentration, the content of p-tert-butylbenzoic acid increased, the concentration of nitric acid decreased to about 10%. When the temperature reached 180e, the content reaches the highest value. When the concentration of nitric acid was higher than 50%, we couldn’t obtain the desired product. In addition, in this experiment, it could also be seen the impact of temperature on the product. The content in the series of high temperature was significantly higher than that of the low temperature series.
  • The effect of reaction temperature on the product
Considering the effect of reaction temperature, we selected the concentration of nitric acid at 10%. The effect of temperature on the product was that the reactant could not get the desired product at the reflux temperature. With the increase of temperature, the product content exhibits an increasing trend. At 170e, the content reaches the highest value with further increasing the temperature having almost no effect on the content.
  • The effect of reaction time on the reaction
A large number of experiments have found that the reaction time only affects the reaction conversion rate, without affecting product selectivity. That is, it does not affect the content of the product and only affects the yield of the product. In the experiment, it can be clearly seen of that the reaction time is not enough when the reactor floating above a layer of liquid organic matter, the analysis is the raw material of tert-butyl toluene.
From the analysis of the data, we can see that the reaction temperature has the greatest influence on the yield. Considering various factors, we selected the reaction conditions as: the temperature: 180e, reaction time: 8h and nitric acid concentration: 10%. According to this condition, the content of p-tert-butylbenzoic acid was 98.4% and the yield was 95.5%.

Application

Important intermediates for organic synthesis.

Chemical Properties

CLEAR COLOURLESS TO YELLOW LIQUID

Uses

Methyl 4-tert-butylbenzoate was used in the synthesis of tris(4-tert-butylphenyl)methyl chloride.

Synthesis Reference(s)

Tetrahedron, 42, p. 553, 1986 DOI: 10.1016/S0040-4020(01)87454-8

General Description

Methyl 4-tert-butylbenzoate undergoes Claisen condensation reaction with 4-methoxyacetophenone to give avobenzone, an ingredient of sunscreen products.

Methyl 4-tert-butylbenzoate Preparation Products And Raw materials

Raw materials

Preparation Products

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Methyl 4-tert-butylbenzoate Suppliers

Shaanxi Coal Chemical Industry Technology Research Institute Co., Ltd.
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TCI (Shanghai) Development Co., Ltd.
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View Lastest Price from Methyl 4-tert-butylbenzoate manufacturers

Hebei Zhuanglai Chemical Trading Co.,Ltd
Product
Methyl 4-Tert-Butylbenzoate 26537-19-9
Price
US $75.00-20.00/kg
Min. Order
1kg
Purity
99%
Supply Ability
20ton
Release date
2024-06-03
Hebei Chuanghai Biotechnology Co,.LTD
Product
Methyl 4-tert-butylbenzoate 26537-19-9
Price
US $10.00/KG
Min. Order
1KG
Purity
99%
Supply Ability
10 ton
Release date
2024-08-21
Hebei Kingfiner Technology Development Co.Ltd
Product
Methyl 4-tert-butylbenzoate 26537-19-9
Price
US $0.00-0.00/kg
Min. Order
1kg
Purity
99%
Supply Ability
50000kg
Release date
2024-05-11

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