Category: 2688-84-8

Synthetic Route of 2688-84-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2688-84-8 name is 2-Phenoxyaniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

In a 50L double-layer cryostat equipped with mechanical stirring, 5 kg was added (due to batch reaction,A plurality of reactors are simultaneously carried out, so that the amount of the raw materials is sufficient to meet the requirements of the step. 2-Aminodiphenyl ether prepared in the above step (2), 30 L of acetonitrile, and the temperature in the autoclave is lowered to -10 C.4.80 Kg of N-bromosuccinimide was added in three portions, and the reaction was carried out for 2 hours.The mixture is distilled to recover acetonitrile, and then 15 L of water is added to the concentrate.15 L of dichloromethane, stirred and separated, and the organic phase was distilled to recover dichloromethane.Drying again gave a brown solid of 7.06Kg.The product was identified as 1-amino-5-bromodiphenyl ether by 1H-NMR and 13C-NMR.The yield was 99%, and the purity of the product was 98% by liquid chromatography.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Phenoxyaniline, and friends who are interested can also refer to it.

Reference:
Patent; Xinxiang Runyu New Materials Technology Co., Ltd.; Geng Weizhi; Zhou Yi; Li Heng; Zhang Yinlong; Ma Chenyang; (18 pag.)CN109942527; (2019); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2688-84-8, name is 2-Phenoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 2688-84-8

To a 1 L four-necked round bottom flask equipped with a stirrer, a Liebig condenser fitted with a calcium chloride tube, a nitrogen inlet tube, a 50 mL isobaric dropping funnel and a thermometer, 50.0 g (0.6 mmol) of 2′-phenoxyaniline was added. 27 mol) and 500 mL of DCM, and the mixture was stirred at room temperature under a nitrogen stream. Subsequently, 42.8 g (0.41 mol) of triethylamine was added, and the mixture was cooled to -10 C. with an ice water bath, and 30.3 g (0.38 mol) of acetyl chloride was added dropwise from the dropping funnel at 0 C. or less while paying attention to heat generation . The mixture was further stirred at the same temperature for 30 minutes, returned to room temperature, and allowed to react after 5 hours to obtain a reaction solution.Next, 250 g of pulverized ice was added to a 1 L four-necked round bottom flask equipped with a stirrer, a Liebig condenser fitted with a calcium chloride tube, a 1 L dropping funnel and a thermometer, and while stirring, the above reaction solution The whole amount was added dropwise. Next, the dropping funnel was washed with 100 mL of DCM and added to the reaction solution, followed by stirring at room temperature for one day and night.The obtained reaction solution was transferred to a 1 L separating funnel, the organic layer was separated, washed three times with 250 mL of water, dried with magnesium sulfate, magnesium sulfate was suction filtered and removed, And the solvent was distilled off to obtain 73.2 g (yield 119.8%) of the target compound. The obtained compound was directly used for the next reaction.

The synthetic route of 2688-84-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; YAMAGATA UNIVERSITY; CHEMIPRO KASEI KAISHA LIMITED; KIDO, JUNJI; SASABE, HISAHIRO; TAKAHASHI, JUN; NAGAI, NAGAI; (723 pag.)JP2018/90561; (2018); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 2688-84-8, name is 2-Phenoxyaniline, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2688-84-8, Recommanded Product: 2-Phenoxyaniline

General procedure: The mixture of intermediate Bn-2 (1 eq.), PTSA*H20 (i72.5 g, 3 eq) inAcetonitrile (224 ml, 1.3 M) was cooled to 5 C. using a ice bath. NaNO2 (41 .7 g, 2 eq.) in 240 ml water was added dropwise. Afier the addition was finished, the mixture was kept at 5 C. for i hr. The resulting diazonium salt was treated slowly with KI (iOO g, 2 eq.) in 300 ml watet After the completion of the reaction, the residue was extracted with EtOAc and the combined organic layer was washed with a iO% Na2SO3(0q) and then dried over Na2504. The organic layer was concentrated under reduced pressure afier filtration. The crude mixture was purified by silica-gel column chromatography to obtain intermediate Bn.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Phenoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NICHEM FINE TECHNOLOGY CO., LTD.; WU, Hui-Ling; LIAO, Liang-Di; SHIEH, Shwu-Ju; CHEN, Chi-Chung; (145 pag.)US2018/155312; (2018); A1;,
Ether – Wikipedia,
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Reference of 2688-84-8, These common heterocyclic compound, 2688-84-8, name is 2-Phenoxyaniline, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

2-Phenoxyaniline (30 mmol) and triethylamine (31.5 mmol) were dissolved in 100 mL of tetrahydrofuran, and the concentration of 2-phenoxyaniline was 0.3 mol/L. The mixture was cooled in an ice-water bath, and stirred. Then oxalyl chloride (15.8 mmol) was added dropwise. The system turned to turbid and triethylamide hydrochloride was formed. The ice-water bath was then removed and the mixture was warmed to room temperature in the air, and continuously stirred for 2 hours until 2-phenoxyaniline was completely consumed (monitored by TLC). Then the stirring was stopped for post process. The stirring bar was removed by a magnetic bar, and tetrahydrofuran was removed by evaporation under reduced pressure. 50 mL of distilled water was added to the resultant residue. The solid on the flask wall was scraped off and immersed into distilled water, and stirred to form slurry. Et3N.HCl was completely dissolved in water while the oxalic diamide was left undissolved. Then the slurry was filtered under reduced pressure, and the solid on filter paper was washed with cold diethyl ether. The residue was removed and dried in an infrared oven, and then dried with an oil pump to afford a white solid (5.45 g, 86% yield). 1H NMR (400 MHz, CDCl3) delta 9.96 (s, 2H), 8.46 (dd, J=8.0, 1.7 Hz, 2H), 7.43-7.30 (m, 4H), 7.22-7.01 (m, 10H), 6.89 (dd, J=8.0, 1.5 Hz, 2H); 13C NMR (100 MHz, CDCl3) delta 157.36, 156.06, 146.73, 129.97, 127.97, 125.40, 124.18, 123.75, 120.49, 119.02, 117.60; HRMS (ESI) calcd. for C26H21N2O4 (M+H)+: 425.1496, Found: 425.1492

The synthetic route of 2688-84-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CE Pharm CO., LTD; Ma, Dawei; Zhou, Wei; Fan, Mengyang; Wu, Haibo; Yin, Junli; Xia, Shanghua; (73 pag.)US10500577; (2019); B2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 2688-84-8,Some common heterocyclic compound, 2688-84-8, name is 2-Phenoxyaniline, molecular formula is C12H11NO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

2-phenoxyaniline (25.0, 0.135 mol) and 30 ml of hydrochloric acid were added to a 1 L round bottom flask reactor, and the mixture was cooled to 0 C and stirred for 1 hour.75 ml of an aqueous solution of sodium nitrite (11.2 g, 0.162 mol) was added dropwise to the reaction solution at the same temperature, followed by stirring for 1 hour.When the aqueous solution of potassium iodide (44.8 g, 0.270 mol) was added dropwise, the temperature of the reaction solution was prevented from exceeding 5 and dropping.The mixture was stirred at room temperature for 5 hours and washed with an aqueous sodium thiosulfate solution after completion of the reaction, followed by extraction with ethyl acetate and water.The organic layer was separated and concentrated under reduced pressure, and then purified by column chromatography to obtain Intermediate 5-a (22.6 g, 56.5%).

The synthetic route of 2688-84-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC Co., Ltd.; Che Chunxu; Po Xipei; Po Shangyu; Shen Youna; Jin Xida; (130 pag.)CN107207454; (2017); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 2688-84-8, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 2688-84-8, name is 2-Phenoxyaniline, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Unless noted, the reaction was carried out as following: to a solution of 1, 4-dioxane (1.0 mL)was added 1,3-Diphenylpropenes 1 (0.1 mmol), nitrogen-based nucleophiles 2 or 4 (0.12 mmol)and oxidant (0.14 mmol). The reaction mixture was stirred at room temperature for 2-5 h and thenthe solvent was removed under vacuum. The residue was purified by column chromatography onsilica gel to yield the desired products.

The chemical industry reduces the impact on the environment during synthesis 2-Phenoxyaniline. I believe this compound will play a more active role in future production and life.

Reference:
Article; Wu, Yinuo; Kwong, Fuk Yee; Li, Pengfei; Chan, Alberts. C.; Synlett; vol. 24; 15; (2013); p. 2009 – 2013;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 2688-84-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2688-84-8, name is 2-Phenoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 1.0 equivalent of intermediate Bn-2 and172.5 g (3.0 eq.) of p-toluenesulfonic acid hydrate (PTSA*H2O) was mixed in 224 ml of a 1.3 M acetonitrile (ACN) solution and cooled to 5 C in an ice bath.41.7 g (2 equivalents) of sodium nitrite (NaNO2) was dissolved in 240 ml of water and added dropwise.After the completion of the dropwise addition, the ice bath at 5 C was maintained for 1 hour, and the aqueous solution of the diazonium salt after the reaction was treated with 100 g (2 equivalents) of potassium iodide (KI) in 300 ml of an aqueous solution, followed by extraction with ethyl acetate. The combined organic phases were washed with aq. 10% aqueous sodium sulphate and dried over sodium sulfate, and then filtered and evaporated. The chemical structural formula of the reactant An for synthesizing the intermediate Bn (especially referring to the intermediates B1 to B4) and the chemical structural formulas and yields of the intermediates Bn-1, Bn-2 and Bn are listed in Table 2-1.

The synthetic route of 2-Phenoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NICHEM FINE TECHNOLOGY CO., LTD.; LU, TAI-NI; WU, HUI-LING; SHIEH, SHWU-JU; CHEN, CHI-CHUNG; (84 pag.)TWI644912; (2018); B;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem