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Valeric Acid CAS 109-52-4

Molecular Formula: C5H10O2

Formula Weight: 102.13

ZSpharmac: Valeric Acid Supplement

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Product Name: Valeric Acid
CAS No: 109-52-4
Purity: 99%

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Basic Info

Product Name:Valeric Acid
Other Names:Valeric Acid, 99%
CAS:109-52-4
Place of Origin:Shandong, China
Brand Name:ZSpharmac
Type:Cosmetic Raw Materials
Appearance:Clear Colorless to Pale Yellow Liquid
EINECS No.:203-677-2
Storage:Store Below +30°C.
Provide:Valeric Acid MSDS;
Valeric Acid COA

What is Valeric Acid?

Valeric Acid is an essential chemical basic material, typically called andrographis oxalic acid. N-valeric acid is generally made use of in the manufacturing of valeric acid esters, as well as is widely made use of in fragrances, medicines, lubricants, plasticizers and other sectors. It is a commonly made use of chemical resources.

At present, the methods for producing Valeric Acid in industry mainly include n-pentanol, n-valeraldehyde oxidation method or reaction with formic acid and 1-butene. The n-amyl alcohol oxidation method requires a large amount of oxidant, which causes serious corrosion to equipment and high production cost. Formic acid is highly acidic and highly corrosive to equipment. In addition, the method of synthesizing n-valeric acid in the laboratory also uses n-butyllithium to react with dry ice. But n-butyllithium is not only expensive, but also dangerous. It has a strong irritating effect on eyes, skin, mucous membranes and upper respiratory tract, and can even cause chemical burns. At the same time, the activity of n-butyllithium is also high, difficult to control, easy to burn and even explode, so it is not suitable for large-scale industrial production. The laboratory method for synthesizing Valeric Acid is also to prepare Grignard reagent from bromobutane, which is then reacted with dry ice. However, the cost of bromobutane is relatively high, and 1,2-dibromoethane or iodine needs to be added as an initiator when bromobutane prepares Grignard reagent, which increases the cost and is not suitable for industrial production.

Valeric Acid Property

Melting point 

−20-−18 °C(lit.)

Boiling point 

110-111 °C10 mm Hg(lit.)

density 

0.939 g/mL at 25 °C(lit.)

vapor density 

3.5 (vs air)

vapor pressure 

0.15 mm Hg ( 20 °C)

refractive index 

n20/D 1.408(lit.)

Fp 

192 °F

storage temp. 

Store below +30°C.

solubility 

40g/l

form 

Liquid

pka

4.84(at 25℃)

color 

Clear colorless to pale yellow

PH

3.95(1 mM solution);3.43(10 mM solution);2.92(100 mM solution);

Odor Threshold

0.000037ppm

explosive limit

1.8-7.3%(V)

Water Solubility 

40 g/L (20 ºC)

 

 

Valeric Acid Uses

  1. Valeric Acid is made use of in spices. Primarily used to prepare flavors such as lotion, cheese, butterscotch, strawberry and also rum.
  2. Valeric Acid is generally utilized in the production of valeric acid esters as raw materials for spices. The raw material of estrogen medication estradiol valerate and disinfectant.
  3. Valeric Acid is utilized in the production of cooling agents (CFC choices), polyol esters of artificial lubricating substances for electric motors and also jet engines, esterified with reduced alcohols as solvents and also as scents and also perfumes, also in the production of crop defense products.
  4. Valeric Acid is made use of as the basic resources for organic synthesis, and is widely used in fragrances, medicines, lubricants, plasticizers and also various other sectors.

Valeric Acid Invention Contents

In order to solve the problems in the prior art, the embodiments of the present invention provide a method for producing Valeric Acid. The technical solution is as follows:

On the one hand, a method for producing Valeric Acid is provided, which is characterized in that, comprising the following steps:

(1) Preparation of Grignard reagent: a part of 1-chlorobutane is added to the mixture of metal magnesium and solvent, after heating to initiate the reaction, the remaining 1-chlorobutane is added dropwise in 3 ~ 10min, and the reaction system is maintained at reflux Under the state, after the 1-chlorobutane is dripped, the reaction system is continued to reflux until the reaction is completed, and wherein the mol ratio of 1-chlorobutane and magnesium is (1~20): 9, the 1-chlorobutane that the first part adds Alkane is (22~24)% of 1-chlorobutane total amount, and described solvent is tetrahydrofuran or ether, and the volume ratio of solvent and 1-chlorobutane is (4~5): 1;

(2) (1) gained reaction mixture is added dropwise in the reaction vessel that dry ice is housed in 10~30min, after dripping is completed, naturally rise to room temperature, add MHSO subsequently , stir, after the reaction is complete, suction filtration, and the filtrate is acidified After purification, n-valeric acid is obtained, wherein the magnesium added in (1): the dry ice added in (2): MHS0 = 9:27:7, and M is K or Na.

Preferably, in the step (1), the 1-chlorobutane added in the first part is 23% of the total amount of 1-chlorobutane.

Preferably, in the step (1), the mol ratio of 1-chlorobutane and magnesium is 1: (1.4~1.6), more preferably 2: 3.

Preferably, the step (1) is carried out under the protection of an inert gas. Since the Grignard reagent will be consumed by air and water, it will affect the reaction effect, such as nitrogen or argon.

Preferably, in the step (2), the purification refers to acidifying the filtrate to a pH value of (3~4), then extracting the acidified filtrate with ether, merging and drying the organic phases, and finally removing the ether to obtain The Valeric Acid. Usually, the reagent added during acidification is 2 mol/L dilute hydrochloric acid or 1 mol/L dilute sulfuric acid.

More preferably, the M is K.

More preferably, the solvent is tetrahydrofuran.

In the described step (1), a part of the 1-chlorobutane that was added earlier can be used as an initiator to initiate a reaction, and after the reaction is initiated, heat is released, and the reaction system is boiled, and the solvent begins to flow back. As a known technique, the initiation reaction needs to be properly heated to facilitate the initiation of the initiation reaction. Then in 3~10min (preferably 4~6min, for example 5 minutes) remaining 1-chlorobutane can be added dropwise, if the reaction is violent, the rate of addition should be properly controlled to maintain the reaction system in a reflux state. Obviously, this step temperature of reaction is relevant with the boiling point of concrete solvent, when solvent adopts tetrahydrofuran, the temperature of reaction of step (1) is controlled at 25 ℃~reflux temperature, namely before dripping remaining 1-chlorobutane, temperature of reaction is in 25 ℃~reflux temperature, after dripping remaining 1-chlorobutane, temperature of reaction is then basically stable at reflux temperature. After the remaining 1-chlorobutane is added dropwise, the required reaction time can be determined by those skilled in the art through experiments, preferably 1 ~ 3h, such as 2h.

In the described step (2), the (1) gained reaction mixture is added dropwise to the reaction vessel equipped with dry ice in 10~30min, for example the time for adding is 30 minutes.

As common knowledge in the art, the preparation of Grignard reagent needs to be carried out under anhydrous conditions, so the reaction raw materials need to ensure anhydrous, and water removal treatment can be used in advance. For example, 1-chlorobutane is frozen and deiced before being put into the reaction.

Embodiments of Valeric Acid

The round base three-necked flask is geared up with a mixing device, a reflux condenser, a consistent pressure going down channel, and a % defense device. To the there-necked flask was included Mg (2.16 g, 90 mmol), completely dry THF (30 mL). 1-Chlorobutane (1.5 mL) was included in the system, adhered to by heating to start the response. After successful initiation, the continuing to be 1-chlorobutane (5.0 mL) was added dropwise to the system within 5 minutes, and also the response system was kept in a reflux state. After the 1-chlorobutane was added dropwise, home heating made the reaction system continue to reflux for 2 hrs, as well as the ready butyl Grignard reagent was directly utilized in the next action reaction without purification.

The round base two-necked container is furnished with a mixing tool, a continuous pressure going down funnel, and an N2 defense tool. Dry ice (270 mmol) was contributed to the two-necked flask, as well as the butyl Grignard reagent prepared above was gradually added dropwise thereto. After the dropwise enhancement was finished within 30 minutes, it was naturally increased to space temperature level, after that KHS0 (90 mmol) was added to the system, mixed for about 30 minutes and then filtered with suction. The filtrate was acidified with 2mol 1/L of weaken hydrochloric acid, gotten used to pH=3-4, and after that the item was extracted with ether to complete. The essences were combined and dried out with a desiccant. The desiccant was eliminated by suction filtering, as well as the ether was focused and also vaporized to obtain pure Valeric Acid with a return of 85%.

Company Profile and Corporate Culture

Company Profile:

ZhiShang Chemical is owned by ZhiShang Group is a professional new-type chemicals enterprise combined into research and development, production and sales .

The company’s competitive product is pharmaceutical raw materials and intermediates (especially carbohydrate derivatives Series), In recent years, the company has made a major breakthrough in food and feed additives, plant extraction, industrial chemicals industry .

The company insists on the spirit of “sincere management, strict quality control, customer as god” , get consistent high praise from customers at home and abroad.

Corporate Culture:

OUR MISSION
Help China Chemicals to benefit the happiness of human life
OUR VISSION
Become the most trusted chemical supplier in the world
OUR BUSINESS PHILOSOPHY
Striver – oriented, enrich employees, customer first, deep service, seek development
OUR VALUES
Be prepared for danger in times of peace, forge ahead actively, unity and cooperation, and be brave to fight

About Us

The production base is located in Zhangqiu chemical industry park and Tai’an high-tech chemical industry park. laboratory and workshop in strict accordance with the GMP standard and the product fit national ISO9001 and ISO2000 standards.

“Zhishang” products are exported to Europe, North and South America, the Middle East, Asia Pacific and Africa area, so as to establish a long-term and stable cooperation relationship with customer in the world.

Company Info
  • Business Type: Manufacturer
  • Product Range: Additive , Chemical Auxiliary & Catalyst , Organic Chemicals
  • Products/Service: Organic Intermediate,Inorganic Chemistry, APIs, Dyestuffs And Pigments, Fragrance And Spices, Food Additives
  • Total Employees: 51~100
  • Capital (Million US $): 10000000RMB
  • Year Established: 2016
Production Capacity
  • No. of Production Lines : 8
  • No. of QC Staff : 5 -10 People
  • OEM Services Provided : yes
  • Factory Size (Sq.meters) : 3,000-5,000 square meters
  • Certificate: ISO9001 , CE , GMP , API , MSDS
  • Factory Location : Diao Town Industry Park, Zhangqiu City, Jinan City, Shandong Province, China.

Service

Pre-Sales Service

* Prompt reply and 24 hours online, professional team to provide best price and high quality product.

* Sample testing support.

* Every batch of products will be tested to ensureits quality.

*The packing also can be according the customers` requirment.

*Any inquiries will be replied within 24 hours.

*we provide Commerical Invoice, Packing List, Bill of loading, COA , Health certificate and Origin certificate. If your markets have any special requirements, let us know.

 

After-Sales Service

*The fact of logistics information monitoring.

* Any questions about the product can be consulted at any time.

*Product has any problem can return.

FAQ

Do you accept sample order?

We will make samples before mass production, and after sample approved, we’ll begin mass production. Doing 100% inspection during production, then do random inspection before packing.

 

HOW TO CONFIRM THE PRODUCT QUALITY BEFORE PLACING ORDERS?

You can get free samples for some products,you only need to pay the shipping cost or arrange a courier to us and take the samples. You can send us your product specifications and requests,we will manufacture the products according to your requests.

What’s your MOQ?

Our MOQ is 1kg. But usually we accept less quantity such as 100g on the condition that sample charge is 100% paid.

Do you supply product report?

Yes. We’ll give you product analysis report before shipping.

  Is there a discount?

Different quantity has different discount.

Shipping

1. ≤50kg, Express delivery recommended, usually called as DDU service;

2. ≤500kg, Air shipping recommended, usually called as FOB, CFR, or CIF service;

3. >500kg, sea shipping recommended, usually called as FOB, CFR, or CIF service;

4. For high value products, please select air shipping and express delivery for safe.

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