Category: iodides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 6940-76-7, name is 1-Chloro-3-iodopropane, 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 6940-76-7, HPLC of Formula: C3H6ClI

A reaction flask or vial was charged 4H-benzo[1,4]ox- azin-3-one (1.0 equiv) dissolved in DMF (0.1 g/ml), Cs2CO3(1.5 equiv) and 1 -chloro-3-iodopropane (1.1 equiv). The reaction was stirred in rt for 60-70 h and evaporated to dryness. The reaction was redisolved in H20 and extractedwith EtOAc 3×1 50 ml. The combined organic phases weredried over Na2SO4 and concentrated to a crude that was useddirectly or purified by column chromatography (heptanes/ EtOAc).5,7-Difluoro-4H-benzo[ 1 ,4]oxazin-3-one (0.24 g, 1.3 mmol), Cs2CO3 (1.08 g, 3.3 mmol), and 1-chloro-3-iodo- propane (0.296 g, 1.45 mmol) were mixed according to GP2.Purified by column chromatography (Si02 heptanes/ EtOAc, gradient 0 to 30% EtOAc) to give the title compound (0.17 g, 49%). R1=0.66 (heptanes/EtOAc 1:1); ?H NMR (CDC13) oe 6.67-6.58 (m, 2H), 4.55 (s, 2H), 4.16-4.10 (m, 2H), 3.59-3.52 (m, 2H), 2.21-2.10 (m, 2H).

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, 1-Chloro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ACADIA PHARMACEUTICALS, INC.; Skjaerbaek, Niels; Koch, Kristian Norup; Friberg, Bo Lennart Mikael; Tolf, Bo-Ragnar; (70 pag.)US9522906; (2016); B2;,
Iodide – Wikipedia,
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Synthetic Route of 5471-81-8, The chemical industry reduces the impact on the environment during synthesis 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, I believe this compound will play a more active role in future production and life.

(a) Synthesis of methyl 3-methyl-4-(3-ethyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyloxy)benzoate In a manner similar to Example 1(a), by the reaction of 2.1 g (8.7 mmol) of 3-ethyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthol with 2 g (7.2 mmol) of methyl 3-methyl-4-iodobenzoate, 2.18 g (79%) of the expected methyl ester was obtained in the form of a pale yellow oil.

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, Methyl 4-iodo-3-methylbenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Centre International de Recherches Dermatologiques Galderma; US6162815; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 69113-59-3, These common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, 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.

General procedure: Aryl iodide or bromides (1 mmol), ArOH (1 mmol), CuI(20 mol%), and dimethyl di (2-pyridyl)silane (20 mol%) were placed in a small round-bottom flask. DMF (3 mL) and K2CO3(276 mg, 2 mmol) were then added together. The mixture was stirred for 24 h at 100C in nitrogen atmosphere. The reaction mixture was cooled to room temperature. Ethyl acetate(10 mL) and H2O (1 mL) were added and the mixture was stirred. The organic layer was separated and the aqueous layer was extracted twice more with ethyl acetate (10 mL). Combined organic layer was dried overNa2SO4 and filtered. The filtrate was concentrated and the resulting residue was purified by silica gelchromatography and afforded the desired products.

The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Baohua; Shi, Lanxiang; Guo, Ruixia; Liu, Sijie; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 191; 6; (2016); p. 930 – 932;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 156150-67-3, name is 2-Chloro-1-fluoro-4-iodobenzene, molecular formula is C6H3ClFI, 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. category: iodides-buliding-blocks

A round bottom flask is charged with 2-sulfanyl-N-(2,2,2-trifluoroethyl)acetamide (example 14, Step 3, 7.69 g), cesium carbonate (19.7 g), dimethylformamide (100 ml) then the suspension is stirred for 30 min at rt. A solution of 3-chloro-4-fluoroiodobenzene (7.69 g) in dimethylformamide (50 ml) was added and the mixture is stirred at room temperature for 12 hours then 1 hour at 70C. The mixture was diluted with ethyl acetate (100 ml) then washed with water (5*100 ml), 2N hydrochloric acid solution, brine, then dried over sodium sulphate. The solvent was removed under reduced pressure to dryness to afford the crude as yellow solid (13 g). The residue was purified by flash column chromatography of the residue (ethyl acetate / heptanes) afforded the title product as a yellow solid (900 mg). lU NMR (400Mz, CDC13): delta 3.70 (s, 2H), 4.40 (m, 2H), 6.90 (d, 2H), 6.95 (br s, 1H), 7.48 (d, 2H), 7.76 (d, 2H). LCMS (Method E) RT 1.03 min, [M+H]+ 408/410.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 156150-67-3, its application will become more common.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; CASSAYRE, Jerome Yves; EL QACEMI, Myriem; LUKSCH, Torsten; RENOLD, Peter; WO2012/156400; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 116632-39-4,Some common heterocyclic compound, 116632-39-4, name is 5-Bromo-2-iodotoluene, molecular formula is C7H6BrI, 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.

General procedure: To a stirred solution of 6-bromo-3-pyridyl boronic acid (1.25 equiv, 847 mg, 4.20 mmol) in 1,4-dioxane (30 mL) under nitrogen were added 5-bromo-2-iodotoluene (1 g, 3.36 mmol) and tetrakis-(triphenylphosphine)palladium(0) (0.05 equiv, 195 mg, 0.17 mmol). After 5 min of stirring, aqueous Na2CO3 (2.5 equiv, 892 mg, 8.42 mmol) in 5 mL of water was added. Then the mixture was heated to 80 C until the starting material was consumed (TLC). After cooling down to room temperature, the mixture was filtered on Celite and washed with CH2Cl2. The aqueous layer was extracted with EtOAc (2×50 mL). Combined organic layers were washed with saturated aqueous solution of NaCl (50 mL), and dried over MgSO4. Solvent was removed in vacuo and crude product was purified by column chromatography, with 99:1 cyclohexane/EtOAc affording 3c as a white solid (520 mg, 47%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Bromo-2-iodotoluene, its application will become more common.

Reference:
Article; Perato, Serge; Voisin-Chiret, Anne Sophie; Sopkova-De Oliveira Santos, Jana; Legay, Remi; Oulyadi, Hassan; Rault, Sylvain; Tetrahedron; vol. 68; 7; (2012); p. 1910 – 1917;,
Iodide – Wikipedia,
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Related Products of 181765-86-6, The chemical industry reduces the impact on the environment during synthesis 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, I believe this compound will play a more active role in future production and life.

Methyl 5-bromo-2-iodobenzoate (500 mg, 1.47 mmol), phenylboronic acid (197 mg, 1.61 mmol), Pd(OAc)2(16.5 mg, 0.0733 mmol), and triphenylphosphine (38.5 mg, 0.147 mmol) were dissolved in a solution of 2M aqueous Na2S04(2.5 mL) and acetone (6 mL). The mixture was degassed with N2for 7 minutes then heated at reflux for 18 hours. The reaction mixture was diluted with EtOAc (100 mL) and washed with brine (100 mL).The organic phase was dried over anhydrous Na2S04and concentrated under reduced pressure. Purification by flash column chromatography (hexanes to 90: 10 hexanes/EtOAc) afforded 10a as a clear oil (326 mg, 76% yield). Rf= 0.47 (hexanes/EtOAc 90: 10 v/v). ‘ H NMR (400 MHz, CDCl3) delta 7.99 (d, .7= 2.1 Hz, 1H), 7.67 (dd; J= 8.2, 2.1 Hz; 1H), 7.45-7.38 (m, 3H), 7.32-7.27 (m, 3H), 3.67 (s, 3H).13C NMR (101 MHz, CDCl3) delta 167.8, 141.5, 140.2, 134.3, 132.8, 132.5, 132.4, 132.4, 128.3, 127.7, 121.2, 52.4. MS (ESI+) calcd for[Ci4H12Br02]+[M+H]+, 291.0; found 290.9.

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, Methyl 5-bromo-2-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; YALE UNIVERSITY; JORGENSEN, William L.; TRIVEDI-PARMAR, Vinay; (142 pag.)WO2019/178480; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 4387-36-4, name is 2-Iodobenzonitrile, molecular formula is C7H4IN, 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. name: 2-Iodobenzonitrile

Example 100B 2-iodobenzamidine To a mixture of ammonium chloride (14 g) in toluene (200 mL) was added trimethylaluminum (131 mL, 2M mixture in toluene) in portions at 0° C. The mixture was stirred at 0° C. for 30 minutes. 2-Iodobenzonitrile (25 g) was added in one portion at 0° C. The mixture was stirred at 100° C. for 12 hours. The reaction mixture was cooled down to 0° C. and was quenched by addition of 200 mL of methanol. The resulting mixture was filtered. After filtering, the filtrate was concentrated under vacuum to provide the crude product which was precipitated from 500 mL of ethyl acetate to provide the title compound. 1H NMR (400 MHz, dimethyl sulfoxide-d6) delta ppm 9.47 (br s, 3H), 8.00 (m, 1H), 7.55 (m, 2H), 7.34 (ddd, J=7.88, 6.89, 2.21 Hz, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4387-36-4, its application will become more common.

Reference:
Patent; AbbVie Inc.; AbbVie Deutschland GmbH & Co. KG; Brady, Patrick B.; Braje, Wilfried; Dai, Yujia; Doherty, George A.; Gong, Jane; Jantos, Katja; Ji, Cheng; Judd, Andrew S.; Kunzer, Aaron R.; Lai, Chunqiu; Mastracchio, Anthony; Risi, Roberto M.; Song, Xiaohong; Souers, Andrew J.; Sullivan, Gerard M.; Tao, Zhi-Fu; Teske, Jesse A.; Wang, Xilu; Wendt, Michael D.; Yu, Yiyun; Zhu, Guidong; Penning, Thomas D.; (218 pag.)US2019/55264; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 52807-27-9,Some common heterocyclic compound, 52807-27-9, name is 4-Chloro-2-iodoanisole, molecular formula is C7H6ClIO, 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.

Add 4-chloro-2-iodo-anisole (10.9 mL, 75.0 mmol), trimethylsilyl acetylene (15.9 mL, 112.5 mmol), copper (I) iodide (0.29 g, 1.5 mmol), and THF (225 ML, anhydrous) to a dry round bottom flask. Add diisopropylamine (22.1 mL, 157.5 mmol) and dichlorobis (triphenylphosphine) palladium (II) (1.58 g, 2.3 mmol) and stir the mixture at room temperature under N2 overnight. Quench reaction with water and extract with EtOAc (x2). Wash combined organic layers with brine, dry over MGS04 and concentrate to get 24 g of a black oil. Adsorb on SI02 and purify the residue by flash chromatography on silica gel eluting with 0-3% ETOAC/HEXANES to afford (5-chloro-2-methoxy- phenylethynyl) -trimethylsilane (13.7 g, 76%). Add a solution of potassium hydroxide (3. 28 g, 58. 5 mmol) in water (30 mL) dropwise over 25 minutes to a stirred solution of (5-chloro-2-methoxy-phenylethynyl)- trimethylsilane (13.7 g, 57.4 mmol) in methanol (275 mL) and stir at room temperature for 2 hours. Concentrate, add brine to residue, and extract with EtOAc (x2). Dry organic layer over MGS04 and concentrate to get 13 g of a black oil. Adsorb on Si02 and purify the residue by flash chromatography on silica gel eluting with 0-5% EtOAc/hexanes to afford the title compound (8. 98 g, 94%).

The synthetic route of 52807-27-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/19184; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Iodo-5-methylbenzoic acid

Schlenk reaction tube, 5-methyl-2-iodobenzoic acid (0.5 mmol), 3-mercapto 1,2,4-triazole (0.5 mmol), potassium carbonate (0.1 mmol) and HMPA (2 mL). The reaction tube was sealed and reacted in an air atmosphere at 80 C 24 hour. After completion of the reaction, acetic acid (1 ml) was added, stirred at room temperature for 1 hour, then extracted twice with methylene chloride. The organic layer was washed three times with saturated brine. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. And purified by column chromatography to obtain the product 2, its structure and characterization data are as follows

The synthetic route of 52548-14-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chen Dingben; Taizhou University; Huang Ling; Lu Jiaming; (6 pag.)CN104788474; (2017); B;,
Iodide – Wikipedia,
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Related Products of 75581-11-2, The chemical industry reduces the impact on the environment during synthesis 75581-11-2, name is 4-Iodo-1-methoxy-2-methylbenzene, I believe this compound will play a more active role in future production and life.

Step 1 : Preparation of ethyl 2,2-difluoro-2-(4-methoxy-3-methylphenyl)acetateTo a solution 4-iodo-1 -methoxy-2-methylbenzene (commercially available, 1 equiv) and ethyl 2-bromo-2,2-difluoroacetate (2 equiv) in DMF (0.3M) was added Cu powder (3 equiv). The reaction slurry was heated to 80C for 1 .5 days, quenched with saturated NaH2P04 (aq) and extracted with ethyl acetate. The organics were dried over Na2S04 and concentrated under vacuum. The residual was purified via silica gel column chromatography to afford the title product.

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, 4-Iodo-1-methoxy-2-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NOVARTIS AG; CORTEZ, Alex; HOFFMAN, Timothy; LI, Yongkai; WU, Tom Yao-Hsiang; ZHANG, Xiaoyue; WO2015/168279; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com