Iodides-buliding-blocks

88-67-5, 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. 88-67-5, name is 2-Iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Add compound 5 (8.44 g, 34.03 mmol) to a 250 ml round bottom flaskAnd 60ml concentrated sulfuric acid, stir to 60 C and add N-bromosuccinimide(4.82 g, 38.06 mmol), reacted for 2 h, and after cooling to room temperature, the solution was dropped into ice water.Extracted with ethyl acetate, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure.Column chromatography gave 9.54 g of white solidCompound 6, yield 86%.

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

Reference:
Patent; Dalian University of Technology; Wang Shisheng; Li Guangzhe; Liu Liqiang; Zhao Weijie; Guo Xiuhan; Li Yueqing; Wang Xu; Dong Huijuan; (21 pag.)CN110041200; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

624-75-9,Some common heterocyclic compound, 624-75-9, name is 2-Iodoacetonitrile, molecular formula is C2H2IN, 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.

e) To a solution of 7-benzyloxymethyl-8-(4-hydroxyphenyl)-1,3-dipropyl-1,3,7-trihydropurine-2,6-dione (1 g, 2.2 mmol) in tetrahydrofuran (20 ml) was added potassium t-butoxide (0.28 g, 2.4 mmol), and the mixture stirred for 30 minutes at room temperature.iodoacetonitrile (0.38 g, 2.23 mmol) was then added, and the mixture stirred for 16 hours at room temperature.The solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate and passed through a silica gel plug, to provide 7-benzyloxymethyl-8-(4-cyanomethoxyphenyl)-1,3-dipropyl-1,3,7-trihydropurine-2,6-dione, a compound of formula (7)

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

Reference:
Patent; Kalla, Rao; Perry, Thao; Elzein, Elfatih; Varkhedkar, Vaibhav; Li, Xiaofen; Ibrahim, Prabha; Palle, Venkata; Xiao, Dengming; Zablocki, Jeff; US2003/229106; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

624-75-9, Adding a certain compound to certain chemical reactions, such as: 624-75-9, name is 2-Iodoacetonitrile, 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 624-75-9.

The compound obtained in Example 64 (4.6 g, 15.35 mmol) and potassium carbonate (10.6 g, 76.73 mmol) were added to acetone (100 mL) and refluxed for 2 hours. To this reaction mixture was dropwise added iodoacetonitrile (1.34 mL, 18.42 mmol), and refluxed over 2 hours. The acetone was removed by vacuum distillation, and the residue was treated in water (200 mL) and ethyl acetate (200 mL). The organic layer was dried over anhydrous magnesium sulfate and distillated in a vacuum. The concentrate was subjected to column chromatography (silica gel, ethyl acetate-hexane 2:3 v/v) to afford a mixture of 2:1 of regioisomers as yellow oil. These two regioisomers (4.16 g, 80%) were used in the next reaction step without separation.Example 65-2Preparation of 4-(2-chloropyridin-5-yl)-5-(3-methoxy-5-methylphenyl)-pyrazol-1-yl)acetonitrile1H NMR (CDCl3) delta 2.28 (s, 3H), 3.66 (s, 3H), 5.16 (s, 2H), 6.71 (s, 2H), 6.84 (s, 1H), 7.24 (d, J=8.3 Hz, 1H), 7.49 (dd, J=2.3, 5.9 Hz, 1H), 7.70 (s, 1H, 8.32 (s, 1H); 13C NMR (CDCl3) delta 21.57, 39.89, 55.23, 110.80, 113.76, 115.28, 117.76, 121.47, 124.02, 127.24, 129.92, 132.57, 138.58, 140.12, 148.71, 149.92, 151.17, 159.69, 162.33.To a solvent mixture of THF and water (4:1, 10 mL) were added the mixture prepared in Example 65 (400 mg, 1.18 mmol), 2-acetylphenyl boronic acid (023 g, 1.42 mmol), dichlorobis(triphenylphosphine)palladium (II) (41 mg, 0.06 mmol) and potassium carbonate (0.16 g, 1.18 mmol). The reaction system was purged with nitrogen gas for 10 min, and stirred at 70 C. for 12 hours under nitrogen atmosphere. The reaction mixture was cooled at room temperature, washed with ice water (100 mL) and extracted with ethyl acetate (100 mL¡Á3). The organic extract was dried over anhydrous magnesium sulfate and distilled under vacuum. The residue was subjected to prep-TLC using a solvent mixture of ethyl acetate/hexane to purify the desired products.Purification yield by prep-TLC (silica gel, ethyl acetate-hexane, 1:2, v/v): (155 mg); m.p. 176-177 C.; 1H NMR (CDCl3) delta 2.25 (s, 3H), 2.28 (s, 3H), 3.70 (s, 3H), 5.14 (s, 2H), 6.72 (s, 1H), 6.76 (s, 1H), 6.89 (s, 1H), 7.44-7.65 (m, 6H), 7.70 (s, 1H), 8.54 (s, 1H); 13C NMR (CDCl3) delta 21.51, 30.58, 39.79, 55.19, 110.80, 113.82, 115.30, 118.66, 121.54, 121.89, 127.06, 127.63, 128.80, 128.96, 130.02, 130.36, 132.92, 136.56, 138.15, 139.93, 141.68, 148.55, 151.23, 155.76, 159.71, 204.39.

According to the analysis of related databases, 624-75-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LEE, So Ha; Yoo, Kyung Ho; Oh, Chang Hyun; Han, Dong Keun; El-Deeb, Ibrahim Mustafa; Park, Byung Sun; Jung, Su Jin; US2011/15395; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

The chemical industry reduces the impact on the environment during synthesis 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, I believe this compound will play a more active role in future production and life. 3032-81-3

Example 35 3-(3,5-Dichloro-phenylamino)-4-methoxy-N-phenyl-benzamide Prepared according to the procedure of Example 33 using 3-amino-4-methoxy-N-phenyl-benzamide (2.0 g, 8.3 mmol), 3,5-dichloroiodobenzene (4.5 g, 16.5 mmol), potassium carbonate (2.9 g, 21.0 mmol), and copper(I) iodide (0.5 g, 2.6 mmol) to give a gummy residue which was subjected to chromatography on a column of silica gel in dichloromethane to afford the product (0.3 g); m.p. 207-208¡ã C. after recrystallization from ethanol. Calculated for C20H16Cl2N2O2.0.2C2H6O: C, 61.80; H, 4.37; N, 7.07. Found: C, 61.47; H, 4.04; N, 7.08.

The chemical industry reduces the impact on the environment during synthesis 3032-81-3. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Warner-Lambert Company; US6268387; (2001); B1;,
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. 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 5471-81-8

A 3 -Liter round bottom flask equipped with a mechanical stirrer, thermocouple, and addition funnel was charged with 100 g of solid 4-iodo-3-methylbenzoic acid methyl ester and 1.0 L of dry THF. The mixture was cooled to -25 0C, and 218 mL of i-PrMgCl (2M in THF) was added dropwise over 25 min while the internal temperature was maintained at <-15 0C. The batch was kept at <-10 0C for 1 hr after the addition of the Grignard reagent. Analysis of a hydrolyzed aliquot showed greater than 97% deiodination. The reaction was then cooled to about -20 0C and quenched with trimethyl borate (77 g). The trimethyl’ borate reaction is exothermic. The temperature increased to about -4 0C during the addition of the trimethyl borate over a time of about 3 min. The resulting solution was aged for 1 h at <0 0C. The batch was then cooled to about -20 0C and further quenched with 1.0 L of IM H3PO4. This quench was also exothermic, raising the temperature to 3 0C by the end of the quench. The batch was aged at room temperature overnight.The THF was then removed by distillation at < 45 0C under reduced pressure. The product slurry was allowed to cool to room temperature, and then was filtered. The cake was washed with water (3 X 500 ml) and toluene (2 X 250 mL) and then was dried under vacuum with nitrogen sweep for 18 h to give the boronic acid 3 as an off-white crystalline solid. The synthetic route of 5471-81-8 has been constantly updated, and we look forward to future research findings. Reference:
Patent; MERCK & CO., INC.; WO2007/79186; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 29289-13-2, name is 2-Iodo-4-methylaniline, 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. 29289-13-2

The compound 2-iodo-4-methyl-aniline (32.6 g, 0.14 mol) was completely dissolved in 300 mL of chloroform in a nitrogen atmosphere, and bromine (21.9 g, 0.14 mol) was added at 0 C., and stirred for 2 hours. The organic layer was extracted with 300 mL of a 1 molar solution of sodium thiosulphate, and then the organic layer was completely distilled and purified by column chromatography (chloroform / hexane) to prepare Compound 1-B (40.2 g, yield: 92%).

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, 29289-13-2, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; LG Chem, Ltd.; Yoon Hong-sik; Kang Yu-jin; Hong Wan-pyo; Kim Jin-ju; (261 pag.)KR2019/78541; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

121554-10-7, A common heterocyclic compound, 121554-10-7, name is 5-Bromo-2-iodobenzonitrile, molecular formula is C7H3BrIN, 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.

EXAMPLE 112a Preparation of intermediate 5-bromo-2-iodo-benzaldehyde To a solution of 5-bromo-2-iodo-benzomitrile (1.54 g, 5 mmol) in DCM (15 mL) was added a solution of DIBALH (6 mL, 6 mmol) dropwise at 0 C. After the addition, the reaction mixture was warmed to r.t. and stirred for 2 h. Then the mixture was poured into 20 g of ice and 20 mL of 1N HCl, filtered and extracted by DCM (40 mL), washed with aqueous sodium bicarbonate, dried over MgSO4 and concentrated to give crude product (Yield: 1.2 g).

The synthetic route of 121554-10-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ding, Qingjie; Jiang, Nan; Yang, Song; Zhang, Jing; Zhang, Zhuming; US2009/156610; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 31599-60-7, name is 1-Iodo-2,3-dimethylbenzene, 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. 31599-60-7

General procedure: A DMF solution (8mL) of the o-substituted aryl iodide (0.36mmol), the o-bromobenzyl alcohol (0.36mmol) and norbornene (34mg, 0.36mmol) was added under nitrogen to a Schlenck-type flask, containing Pd(OAc)2 (4mg, 0.018mmol), the phosphine (0.036mmol), when required, and K2CO3 (124mg, 0.90mmol) or CsOPiv (211mg, 0.90). The reaction mixture was stirred at 105C for 24h. After cooling to room temperature the organic layer was diluted with EtOAc (20mL), washed twice with water (20mL) and dried over Na2SO4. The solvent was removed under reduced pressure and the resulting residue was purified by flash chromatography on silica gel using mixtures of hexane-EtOAc as eluent.

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, 31599-60-7, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Della Ca, Nicola; Fontana, Marco; Xu, Di; Cremaschi, Mirko; Lucentini, Riccardo; Zhou, Zhi-Ming; Catellani, Marta; Motti, Elena; Tetrahedron; vol. 71; 37; (2015); p. 6389 – 6401;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 612-55-5, name is 2-Iodonaphthalene, This compound has unique chemical properties. The synthetic route is as follows., 612-55-5

General procedure: Benzo[d]thiazole (1.0 mmol), aryl iodide(1.5 mmol), CuFe2O4 nanoparticles (0.05 mmol), ligand (0.02 mmol), and base were (1.5-2 mmol) taken in solvent (3 mL) and heated at 110 oC, for 10 h. The progress of the reaction was monitored by TLC. After the reaction was complete CuFe2O4 nanoparticles were placed on the bottom of the flask by a neodymium magnet, and the supernatant solution was removed. The crude residue was extracted with ethyl acetate (3 10 mL). The combined organic layers were extracted with water, saturated brine solution, and dried over anhydrous Na2SO4. The organic layers were evaporated under reduced pressure and the resulting crude product was purified by column chromatography to give the corresponding 2-phenylbenzo[d]thiazole in excellent yields. The identity and purity of the product were confirmed by 1H, 13C NMR, and mass spectra.

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:
Article; Satish; Reddy, K. Harsha Vardhan; Anil; Ramesh; Kumar, R. Uday; Nageswar; Tetrahedron Letters; vol. 56; 34; (2015); p. 4950 – 4953;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

112671-42-8, 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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows.

mixture of compound 71 (6.5 g, 19.8 mmol) and Fe (4.98 g, 89.2 mmol) inCH3COOH (30 mL) and CH3CH2OH (30 mL), was refluxed for 1.5 hours. The mixture was cooled to room temperature and after addition of saturated NaHC03 (aq.), extracted with ethyl acetate (3 x 150 mL).The combined organic layer was separated, dried over Na2S04 and the solvent was removed in vacuo, resulting in compound 72 (5.9 g). Method A2; Rt: 1.17 min. m/z=: 299.6 (M+H)+ Exact mass: 298.9

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; TIBOTEC PHARMACEUTICALS; VANDYCK, Koen; VERSCHUEREN, Wim Gaston; RABOISSON, Pierre Jean-Marie Bernard; WO2012/13643; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com