4-Methylanisole is an anemic transparent liquid with a solid flower fragrance. It can be obtained by responding p-cresol with dimethyl sulfate in alkaline remedy. It can be made use of to prepare essences such as fabricated yamba, daffodil and so forth. Today, the technique for synthesizing p-methylanisole is mainly to react p-cresol and also methylating reagents, such as dimethyl carbonate (DMC), methyl iodide, dimethyl sulfate (DMS) or such. Wherein methyl iodide is because of Due to its high rate as well as stringent operating requirements, it is not extensively utilized. As a new industrial reagent, DMC is being extensively researched.
0.969 g/mL at 25 °C(lit.)
5.25 mm Hg ( 50 °C)
Sealed in dry,Room Temperature
Clear colorless to slightly yellow
4-Methylanisole can be utilized in a proper quantity in the scent sorts of jasmine grandiflora, white orchid, ylang-ylang, narcissus, daffodil, great smelling Roland, hyacinth and also gorse. It can likewise be used in a percentage for lily of the valley, increased, and lilac. It can be made use of in soap essence with bromostyrene, and also occasionally made use of in food essence, mainly made use of in nut taste, such as walnut as well as hazelnut significance.
4-Methylanisole is a food seasoning that is permitted to be utilized according to GB 2760-96. Primarily utilized to prepare walnut, hazelnut and various other nut flavors.
4-Methylanisole has aromatic violet and fragrance and also ylang blossom scent, which is naturally present in ylang oil and also cananga ylang oil, and is a vital one among comparable ethers. This product is an edible seasoning that is permitted to be made use of according to GB2760-86 of our country. It is primarily utilized to prepare walnut, hazelnut and other nut tastes. This item is additionally utilized to make flavors such as ylang ylang, cananga, violet, narcissus, as well as gorse. It can additionally be utilized as an intermediate for a few other flavors.
Preparation of 4-Methylanisole
Method 1: Use tetrabutylammonium bromide as a stage transfer catalyst to militarize the response of p-cresol and dimethyl sulfate to synthesize 4-Methylanisole. The outcomes show that when the molar proportion of dimethyl sulfate and p-cresol is 1.4, the phase transfer The return of p-methylanisole can reach up to 92.36% under the condition of 6% driver quantity, pH= 8, water bathroom temperature level control 50-60 ℃, as well as response time 6h.
Add 10.5 mL (0.1 mol) of p-cresol and also 30mL of toluene right into a three-necked flask equipped with a magnet, thermometer, dropping funnel, as well as spherical reflux condenser, mix magnetically and warm to 50 ° C in a water bathroom at the same time, include stage Transfer catalyst tetrabutylammonium bromide 1.93 g (0.006 mol), utilize a particular amount of 30% K2CO3 service to readjust the pH to be alkaline, control the temperature level at 50-60 ° C, proceed mixing for 40min, and also slowly decrease (CH3) 2SO4 into the reaction bottle The remedy was 13.23 mL (0.14 mol), as well as the going down time was 50min. At the same time, the pH of the solution was regulated to be 8. After the dropping, the reaction was refluxed at the same temperature level for 6h. After the reaction was finished, the top natural layer was washed with 3 × 20mL10% ammonia water, as well as the aqueous layer was eliminated by splitting up. Clean with saturated NaCl solution till neutral, and dry with anhydrous CaCl2, filter, and boil down under reduced pressure to collect the product. The item yield is 92.36%.
Method 2: a preparation approach of 4-Methylanisole, specifically making up the adhering to steps:
1) Neutralization response: p-cresol: 100.0 g (material: 99.1%, 0.9176 mol), outright ethanol: 600ml, open nitrogen protection, established nitrogen flow: 0.5 l/min. The outer wall surface of the four-necked flask is cooled down with cooling water, and also the inner temperature level is regulated not to exceed 35 ° C. Slowly include salt hydroxide: 37.5 g (0.9375 mol) into the four-necked flask from the thermostat mouth (pull out the thermostat). After feeding, the reaction was mixed for 1.0 hour. After the response is completed, the outer wall surface of the four-neck flask is heated with 85-90 ° C warm water, and also the ethanol is constantly distilled out under the defense of nitrogen. In the later phase of purification, the discharge rate of ethanol will certainly become smaller as well as smaller. When the discharge of ethanol is really small, vacuum cleaner healing is executed, as well as the vacuum cleaner degree is managed to be above -0.08 MPa to recover the ethanol to dry skin. The residue in the four-necked flask is salt p-cresol, amount: 121.1 g, web content: about 98.2%.
2) Methylation reaction 1: In a 500ml four-necked flask outfitted with a thermometer, a mixing paddle as well as a reflux condenser, put the ready salt p-cresol: 50.0 g (material: regarding 98.2%, 0.3777 mol), cyclohexane Alkane: 300ml. The external wall surface of the four-neck flask was kept cozy with 40 ° C warm water, started stirring, and also changed the mixing speed to be more than 500r/min. Weigh dimethyl sulfate: 50.0 g (content: 98.7%, 0.3917 mol) and also participate in the constant stress going down funnel, then drop the dimethyl sulfate in the continuous stress dropping channel to four The methylation reaction was performed in a flask. After the enhancement of dimethyl sulfate is total, maintain the temperature for 5.0 to 8.0 hrs.
3) Post-processing: After warm conservation, filter after cooling down. The filter cake was cleaned with 100ml cyclohexane, and also dried out to acquire sodium methyl sulfate: 50.8 g, material: 97.3%. After the filtrate was cleaned with alkaline water, the solvent was recouped (the washed alkaline water was reused), as well as the solvent recuperation was finished to get 4-Methylanisole: 45.6 g, material: 98.1%, return: 97.0%.
4) Methylation response 2: put into a 500ml three-neck flask furnished with a thermometer, a stirring paddle as well as a reflux condenser: 42.5 g of sodium p-cresol (web content: regarding 98.2%, 0.3210 mol), methyl tetrahydrofuran: 300ml, Dry salt methyl sulfate: 50.8 g (web content: 97.3%, 0.3689 mol). Mixing was started, as well as the outer wall surface of the three-neck flask was warmed with an electrical home heating mantle, and the reaction was refluxed for 5.0 to 8.0 hrs. After the response was finished, it was cooled down to space temperature.
5) Post-processing: After cooling, filter, and the filter cake is constructed from salt sulfate for detailed utilization. The filtrate was transferred to a 500ml three-necked flask to recuperate methyl tetrahydrofuran. After recovery, 4-Methylanisole was obtained: 38.5 g, spotted material: 97.2%, return: 95.5%.
Ecological Information on 4-Methylanisole
The production and also use 4-Methylanisole as a synthetic fragrance, a scent energetic ingredient, and as a starting item for the preparation of p-anisaldehyde might lead to its launch to the setting with different waste streams. 1-Methoxy-4-methylbenzene has been detected in lake water and also sewer, along with in blue cheese scents. 1-methoxy-4-methylbenzene will have minimized flexibility if launched right into dirt. Volatilization of 1-methoxy-4-methylbenzene may be very crucial for both moist as well as likewise dry soil surface areas. There want information to recognize the cost or significance of 4-Methylanisole biodegradation in soil or water. If released into water, 1-methoxy-4-methylbenzene may adsorb to put on hold solids as well as also particles. 1-Methoxy-4-methylbenzene may volatilize from water surface areas with approximated half-lives of 3.4 hrs and likewise 4.4 days for version rivers and also version lakes, especially. The estimated BCF value of 62 suggests just moderate bioaccumulation of 1-methoxy-4-methylbenzene in aquatic bacteria. If launched to the environment, 4-Methylanisole will absolutely exist in the gas phase. Vapor-phase 1-methoxy-4-methylbenzene degrades in the feel by response with photochemically created hydroxyl teams with an approximated half-life of around 14 hours. 4-Methylanisole is launched into the atmosphere with plants emissions. The standard population might be exposed to infected water, the application of scent, and also its existence in food.
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Company Profile and Corporate Culture
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 .
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Factory Location : Diao Town Industry Park, Zhangqiu City, Jinan City, Shandong Province, China.
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