Category: 135050-44-1

Related Products of 135050-44-1, 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. 135050-44-1 name is 3-Chloro-4-iodoaniline, 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.

3-chloro-4-iodoaniline (15 g, 59 mmol) dissolved in diethyl [(ethyloxy)methylene]malonate (19 mL, 95 mmol) and heated at 160 C for 4 hours under a reflux condenser. The condenser was then removed and EtOH evaporated. After one hour, it was cooled to rt to solidify, broken up and the solid was suspended in hexane. The mixture was filtered and the filter cake washed with hexane several times to give a grey solid (23 g, 91%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-4-iodoaniline, and friends who are interested can also refer to it.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BURY, MICHAEL JONATHAN; CASILLAS, LINDA N.; CHARNLEY, ADAM KENNETH; HAILE, PAMELA A.; MARQUIS JR., ROBERT W.; MEHLMANN, JOHN F.; ROMANO, JOSEPH J.; SINGHAUS, JR., ROBERT R.; WANG, GREN Z.; (153 pag.)TWI609011; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3-Chloro-4-iodoaniline

[00675] Example 6: 4-[(aminocarbonyl) amino]-1-(3-chloro-4- iodophenyl)-1 H-pyrazole-3-carboxamide; [00677] Step 1: Preparation of (2E)-2- [ (3-chloro-4- iodophenyl) hydrazono] -2-cyanoacetamide; [00679] A 250 mL 2-neck flask, flushed with N2, was charged with a stir bar and 3-chloro-4-lodoaniline (19.01 g, 75 mmol) and was then cooled in acetone/ice bath to 0C. To this was added conc. HCI (19 mL) dropwise at a rate that maintained the temperature below 5C. Water (60 mL) was added followed by a solution of sodium nitrite (5.175 g, 75 mmol) in water (15 mL) over a 5 min period. After 75 mins, a solution of sodium acetate trihydrate (30.62 g, 225 mmol) in water (75 mL) was added over a 5 min. period with the temperature maintained at 5C. The resultant yellowish slurry was then used as described in the following paragraph. [00680] To a well-stirred solution of cyanoacetamide (12.61 g, 150 mmol) in water (115 mL) and ethanol (75 mL) in a 500-mL round bottom flask was added a solution of acetate trihydrate (10.5 g, 75 mmol) in water (25 mL) and this mixture was cooled to-7C in an acetone/water bath. To this solution was added the slurry from the previous paragraph dropwise over a 70-minute period with the temperature maintained at 0C ( 2C) during the addition. After 2.5 h, the cold mixture was filtered and the solids washed with water (3 X 100 mL) and air-dried. These solids were washed with methanol (4 X 100 mL) and dried in vacuo to give a yellow solid. The methanol washes were concentrated, cooled, and filtered to provide additional product.’H NMR (DMSO-d6) : 5 11.750 (m, 1 H), 7.940 (m, 1 H), 7.860 (m, 1 H), 7.822 (m, 1 H), 7.550 (m, 1 H), 7.330 (m, 1 H). MS (ESI-) for CgH6CIIN40 m/z 347.0 (M-H) -.

The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHARMACIA CORPORATION; WO2005/37797; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-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 135050-44-1, HPLC of Formula: C6H5ClIN

A solution of sodium nitrite (3.27g) in water was added dropwise over 1H to a stirred solution OF 3-CHLORO-4-IODOANILINE (LO. OG) in a mixture of THF (120ML) and concentrated hydrochloric acid (50ml) at-5 TO-1C. Magnesium chloride (6.39g) was then added and the resulting mixture poured into a stirred solution of acetic acid (50ml) saturated with sulfur dioxide and containing cuprous chloride (2.14g). After heating at 34C for 30MIN, the mixture was poured into brine, extracted with EtOAc, washed with aqueous sodium bicarbonate and brine, dried (MGS04) and evaporated. The residue was dissolved in THF (100ml), 0.880 ammonia (100ml) added and stirred for 2h. The mixture was diluted with brine, extracted with EtOAc, washed with brine, dried (MGS04) and evaporated. The residue was treated with isohexane/ether (4: 1) and filtered to give the subtitle compound. Yield 5.67g. 1H NMR DMSO-d6: No. 8.18 (d, 1H), 7.92 (d, 1H), 7.56 (s, 1H), 7.47 (dd, 1H)

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, 3-Chloro-4-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-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 135050-44-1, SDS of cas: 135050-44-1

3-Chloro-4-iodoaniline (3.0 g, 11.8 mmol), (4-chloro-2-methylphenyl)boronic acid (2.4 g, 14.2 mmol), Pd(dppf)Cl2 (1.0 g, 1.2 mmol), and K2CO3 (3.3 g, 23.7 mmol) were dissolved in 1,4-dioxane (40 mL) and water (10 mL) and the resulting mixture was heated to 80 C. After 16 h the resulting mixture was cooled to room temperature, diluted with EtOAc, washed with water and brine, dried (Na2SO4), and dry packed onto silica gel. Column chromatography yielded the title compound.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Chakravarty, Devraj; Kreutter, Kevin; Powell, Mark; Shook, Brian; Song, Fengbin; Xu, Guozhang; Yang, Shyh-Ming; Zhang, Rui; Zhao, Bao-Ping; US2012/302610; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-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 135050-44-1, Recommanded Product: 3-Chloro-4-iodoaniline

EXAMPLE 8 (METHOD 2A) (3-Chloro-4iodo-phenyl)-carbamic acid tert-butyl ester To a solution of 3-chloro-4-iodo-aniline (10 g) in tetrahydrofuran (40 mL) containing diiso-propylethylamine (6.9 mL) is added di-tert-butyl-dicarbonate (8.6 g) and the mixture is heated to reflux. After approximately 15 hours additional portions of diisopropylethylamine (6.9 mL) and di-tert-butyl-dicarbonate (21 g) is added and heating is continued for approximately 24 hours. The solution is then cooled, concentrated under reduced pressure, diluted with ethyl acetate, and washed successively three times with 5% aqueous hydrochloric acid then once with saturated aqueous sodium chloride. The solution is dried over anhydrous sodium sulfate then concentrated under reduced pressure to provide the desired crude product as a brown oil. Crystallization is induced by addition of hexanes, and the collected solid material is recrystallized from hexanes to give the desired product as a white solid.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; American Home Products Corporation; US6166028; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C6H5ClIN

A solution of 3-CHLORO-4-IODO-ANILINE (5. 6G), ISOAMYLNITRITE (8. 8ML) and ETHYLDISULPHIDE (13. 4ML) in acetonitrile (100ml) was heated at 60C for 24h. The solvent was removed under reduced pressure and the residue purified by chromatography on silica eluting with 1% ETHYLACETATE/ISOHEXANE. YIELD 4. 02G ‘H NMR CDC13 : 8 7. 70 (1H, D) ; 7. 36 (1H, d); 6. 87 (1H, dd); 2. 94 (2H, q) ; 1. 32 (3H, t)

The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 135050-44-1

5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (21.15 g, 113.62 mmol) was added to 3-chloro-4-iodoaniline (24 g, 94.69 mmol) in EtOH (450 mL). The resulting solution was stirred at 80 C. overnight. The reaction mixture was filtered and the solid collected washed with diethyl ether (400 mL) to afford 5-[(3-chloro-4-iodoanilino)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione (37 g, 96%) as a white solid; 1H NMR (400 MHz, DMSO, 30 C.) 1.67 (6H, s), 7.34 (1H, dd), 7.90-7.98 (2H, m), 8.57 (1H, s), 11.20 (1H, s).

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, 135050-44-1, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; Kettle, Jason Grant; Bagal, Sharanjeet; Robb, Graeme Richard; Smith, James Michael; Goldberg, Frederick Woolf; Cassar, Doyle Joseph; Feron, James Lyman; US2019/177338; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

135050-44-1, Adding a certain compound to certain chemical reactions, such as: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-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 135050-44-1.

The N-(3-chloro-4-iodophenyl)methanesulphonamide used as a starting material was obtained by the reaction of 3-chloro-4-iodoaniline and methanesulphonyl chloride using a similar procedure to that described in the portion of Example 3 which is concerned with the preparation of N-(4-iodophenyl)methansulphonamide.

According to the analysis of related databases, 135050-44-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Imperial Chemical Industries PLC; ICI Pharma; US5236948; (1993); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-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 135050-44-1, 135050-44-1

STEP A: 2,2′-dichloro-4′-(trifluoromethyl)-[1,1′-biphenyl]-4-amine 3-Chloro-4-iodoaniline (3.0 g, 11.8 mmol), (2-chloro-4-(trifluoromethyl)phenyl)boronic acid (3.2 g, 14.2 mmol), Pd(dppf)Cl2 (969 mg, 1.2 mmol), and K2CO3 (3.3 g, 23.7 mmol) were dissolved in 1,4-dioxane (40 mL) and water (10 mL) and the resulting mixture was heated to 80 C. After 16 h the resulting mixture was cooled to room temperature, diluted with EtOAc, washed with water and brine, dried (Na2SO4), and dry packed onto silica gel. Column chromatography yielded the title compound.

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, 3-Chloro-4-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chakravarty, Devraj; Greco, Michael; Shook, Brian; Xu, Guozhang; Zhang, Rui; US2012/302641; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 135050-44-1, name is 3-Chloro-4-iodoaniline, 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. 135050-44-1

2.75 g (10.8 mmol) of 3-chloro-4-iodoaniline are dissolved in 20 ml of anhydrous dioxane and admixed successively with 4.98 g (13.5 mmol) of the compound from example 92A, 103 mg (0542 mmol) of copper(I) iodide, 4.61 g (21.7 mmol) of potassium phosphate and 116 mul (1.085 mmol) of N,N’-dimethylethylenediamine. The reflux apparatus is inertized by repeated application of a gentle vacuum and flushing with argon. The reaction mixture is heated to reflux for 15 hours. After this time, it is allowed to cool to RT. It is admixed with water and extracted with ethyl acetate. The organic extract is washed successively with water and saturated sodium chloride solution. Then it is dried over anhydrous magnesium sulfate and filtered, and the filtrate is freed of the solvent under reduced pressure. The crude product thus obtained is first purified by suction filtration through silica gel with 20:1?1:4 cyclohexane/ethyl acetate as the eluent. This affords 3.12 g of a still-contaminated product which is purified further by means of preparative HPLC with an acetonitrile/water mixture. This affords 0.71 g (13% of theory) of the title compound. 1H NMR (400 MHz, DMSO-d6, delta/ppm): 7.67-7.62 (m, 4H), 7.48-7.40 (m, 6H), 6.91 and 6.81 (2 d, together 1H), 6.67 and 6.62 (2 d, together 1H), 6.50 and 6.47 (2 dd, together, 1H), 5.41 (s, broad, 2H), 4.08-4.00 (m, 1H), 3.78-3.73 (m, 1H), 3.50-3.41 (m, 1H), 3.40-3.32 (m, 1H, partly obscured by the water signal), 2.07-1.96 (m, 3H), 1.92-1.81 (m, 2H), 1.01 and 1.00 (2 s, together 9H). HPLC (Method 5): Rt=3.26 min. MS (ESIpos, m/z): 493/495 (35Cl/37Cl) (M+H)+.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 135050-44-1.

Reference:
Patent; BAYER SCHERING PHARMA ATIENGESELLSCHAFT; US2010/298293; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com