Month: July 2021

Reference of 5460-32-2,Some common heterocyclic compound, 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, molecular formula is C8H9IO2, 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: Under Oxygen, a reaction tube was charged with p-iodoanisole (46.3 mg, 0.2 mmol), urea (48.0 mg, 0.8 mmol), CuF2 (4.1 mg, 0.04 mmol), L1 (10.8 mg, 0.06 mmol), Li2CO3 (44.3 mg, 0.6mmol) and DMSO (2 mL). The mixture was stirred at 150 oC for 36 h. After the completion of the reaction, monitored by TLC, the solvent was evaporated under reduced pressure and the residue was purified by flash column chromatography on silica gel to give the product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Iodo-1,2-dimethoxybenzene, its application will become more common.

Reference:
Article; Zheng, Kui; Liu, Bin; Chen, Shuyou; Chen, Fan; Tetrahedron Letters; vol. 54; 38; (2013); p. 5250 – 5252;,
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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 328-73-4

Magnesium (230 mg) was added to 3,5-bis (trifluoromethyl) phenyl iodide (3.0 g, 8.8 mmol) in tetrahydrofuran (THF, 80 ml) and stirred for 1-5 hours.The temperature was lowered to -20 ° C and 3.0 g of DMTr-protected propylene oxide (8 mmol) in THF (10 ml) was added. Two hours after the reaction was returned to room temperature for 8 hours. Workup and purification by column chromatography gave 3.73 g of compound 7 (79percent).

The synthetic route of 328-73-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Shanghai Organic Chemistry Institute; Wang Ruowen; Qing Fengling; (27 pag.)CN103880877; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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. Recommanded Product: 13421-13-1

In a MW tube was added 4-chloro-2-iodobenzoic acid (260 mg, 0.92 mmol), 1 H-1 , 2,3- Triazole (0.1 1 ml_, 1 .84 mmol) and (1 R,2R)-N 1 ,N2-dimethylcyclohexane-1 ,2-diamine (0.03 ml_, 0.18 mmol). To these solids were added 1 ,4-Dioxane (1 ml_) and Water (0.1 ml_), then Cul (8.77 mg, 0.05 mmol) and finally Cs2C03 (0.6 g, 1 .84 mmol). The mixture was then warmed to 100 C for 2.5 hrs and left at RT O/N . HCI 6 N was added until pH 2, then volatiles were removed under vacuum and the crude material was purified by RP on C18 column (from H20/CH3CN 95:5 + 0.1 % of FA to H20/CH3CN 5:95 + 0.1 % of FA) affording 4-chloro-2-(2H-1 ,2,3-triazol-2-yl)benzoic acid (p182, 120 mg, y= 58%) as white solid. MS (mlz): 223.9 [MH]+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 13421-13-1, its application will become more common.

Reference:
Patent; CHRONOS THERAPEUTICS LIMITED; MICHELI, Fabrizio; BERTANI, Barbara; GIBSON, Karl Richard; DI FABIO, Romano; RAVEGLIA, Luca; ZANALETTI, Riccardo; CREMONESI, Susanna; POZZAN, Alfonso; SEMERARO, Teresa; TARSI, Luca; LUKER, Timothy Jon; (275 pag.)WO2019/43407; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 618-91-7, name is Methyl 3-iodobenzoate, molecular formula is C8H7IO2, 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. Product Details of 618-91-7

General procedure: Iodides 2 (10.0 mmol), zinccyanide (10.0 mmol), tetrakis (triphenylphosphine) palladium (2.0 mmol) weredissolved in 20 mL DMF. The reaction was heated at 80 oC for 5 hoursunder the protection of N2. The mixture was extracted with CH2Cl2 (25×3 mL) andorganic layers were combined, washed with brine, dried over Na2SO4.The solvent was evaporated under vacuum to give crude product, which waspurified by column chromatography on silica gel to give products 3-1~3-3.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 618-91-7, its application will become more common.

Reference:
Article; Han, Mei; Li, Shan; Ai, Jing; Sheng, Rong; Hu, Yongzhou; Hu, Youhong; Geng, Meiyu; Bioorganic and Medicinal Chemistry Letters; vol. 26; 23; (2016); p. 5679 – 5684;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 626-01-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 626-01-7 as follows.

General procedure: A mixture of substituted aniline (2 mmol), ethyl acetoacetate (1 mmol),RuCl3.3H2O (15 mol%), and ethanol (5 mL) were stirred in a 10 mLround bottom flask at room temperature. After 20 minutes substitutedbenzaldehyde (2 mmol) was added and the reaction mixture was stirredfor the time indicated in Table 3, while being followed by TLC. Aftercompletion of the reaction, the thick precipitate was filtered off andwashed with ethanol (3 × 5 mL) to give the pure product 4.

According to the analysis of related databases, 626-01-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Mohammadi, Sedigheh; Abbasi, Mohsen; Journal of Chemical Research; vol. 39; 2; (2015); p. 123 – 126;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 624-76-0, A common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, molecular formula is C2H5IO, 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.

1.5 equivalents of 2-iodoethanol was added to 2,3,3-trimethylindolenine and refluxed for 18 hours in toluene solvent to obtain intermediate 1. One equivalent of N, N’-diphenylformamidine and one equivalent of triethyl orthoformate was added to Intermediate 1 obtained, and refluxed in an ethanol solvent for 16 hours to obtain Intermediate 2.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Samsung SDI Co., Ltd; Lee Yeong; Kim Gyu-yeong; Choi Eun-jeong; Shin Myeong-yeop; Han Gyu-seok; (43 pag.)KR2018/76149; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 111771-08-5, These common heterocyclic compound, 111771-08-5, name is 2-Fluoro-6-iodobenzoic acid, 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 2-78 4-Chloro-5-fluoro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline Following the procedures described in Reference Example 2-5 and Example 2-1, the title compound was prepared from 2-fluoro-6-iodobenzoic acid and 3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-ylamine (51% yield). mp: 160-161 C. (recrystallized from ethyl acetate). NMR (CDCl3) delta: 3.01 (3H, s), 7.14-7.29 (2H, m), 7.63-7.76 (1H, m), 7.88-8.01 (2H, m), 8.65-8.78 (2H, m).

Statistics shows that 2-Fluoro-6-iodobenzoic acid is playing an increasingly important role. we look forward to future research findings about 111771-08-5.

Reference:
Patent; Uchikawa, Osamu; Mitsui, Keita; Asakawa, Akiko; Morimoto, Shigeru; Yamamoto, Masataka; Kimura, Hiroyuki; Moriya, Takeo; Mizuno, Masahiro; US2003/187014; (2003); 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, A new synthetic method of this compound is introduced below., Product Details of 31827-94-8

A 1 L round bottom flask equipped with a mechanical stirrer, thermocouple, and a reflux condenser was charged with 2′-bromo-4-iodoacetophenone (44.0 g, 0.135 mol), potassium acetate (19.9 g, 0.203 mol), benzyl triethylammonium chloride (1.5 g, 0.007 mol) and 1,2-dichloroethane (425 mL). The reaction mixture stirred at 70 C. for 4 hours then was cooled to 25 C. Water (250 mL) was added and the contents were shaken in a separatory funnel. The dichloroethane layer was separated and was washed with aq. saturated sodium bicarbonate (200 mL) and brine (100 mL). The dichloroethane was dried over sodium sulfate, filtered, and the solvents were removed under reduced pressure to give product as a tan solid (41.2 g, 97% yield): mp 103-107 C.

The synthetic route of 31827-94-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tisdell, Francis Eugene; Bis, Scott Jerome; Hedge, Vidyadhar Babu; Martin, Timothy Patrick; Perreault, Denise Marie; Yap, Maurice Chee Hoong; Guenthenspberger, Katherine Anne; Dripps, James Edwin; Gifford, James Michael; Schoonover, Joe Raymond; Karr, Laura Lee; Dintenfass, Leonard Paul; Neese, Paul Allen; US2004/6108; (2004); A1;,
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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 2043-57-4

15 mL of freshly distilled and dry THF under nitrogen was cooled to -78 C. 4.0 mL of LDA in THF (1 .0 M) (4 mmol) was added quickly. 0.332 mg [1 .8 mmol] of 4,4′-dimethyl-2,2′-bipyridine, dissolved in 3 ml of dry THF, were added and kept under stirring for 30 minutes at – 78 C, then for 15 minutes at -10 C and finally the temperature was cooled again at -78 C for further 15 minutes. Then 1 .896 g [4 mmol] of 1 H,1 H,2H,2H-perfluorooctyl iodide were added. After the addition, the reaction mixture was allowed to warm slowly to room temperature. The reaction was added with 20 ml of brine and extracted with diethyl ether and dried over Na2SO4. Evaporation u.v. (30 C/2.4 kPa) gave a crude product, that was purified by silica gel column chromatography eluting with methanol/dichloromethane solvent mixture, using an appropriate gradient (2:98 final eluting solvent mixture ratio). After removal of the solvent u.v. (30 C/ 2.4 kPa) 0.512 g of the desired compound was obtained as a white solid. 1H-NMR (400 MHz, CDCI3): 8.60 (d, 2H, J=5.1 Hz), 8.28 (s, 2H), 7.16 (dd, 2H, J=1 .6 Hz, J=3.3 Hz), 2.82 (t, 4H, J=7.5 Hz), 2.21 -1 .99 (m, 8H) ppm. 19F-NMR (376.3 MHz, CDCI3): -126.1 , -123.4, -122.8, -121 .9, -1 14.1 , -80.81 ppm.

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 2043-57-4.

Reference:
Patent; TOZZI GREEN S.P.A.; BORZATTA, Valerio; ZAMA, Isabella; RIGHI, Paolo; GORNI, Giacomo; (39 pag.)WO2019/29789; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 766-99-4, name is 1-Ethynyl-4-iodobenzene, 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 766-99-4, Product Details of 766-99-4

4-iodophenylacetylene 114 mg (0.5 mmol), silver nitrite 115.5 mg (0.75 mmol), N-chlorosuccinimide133.5 mg (1.0 mmol) was sequentially added to a 10 mL pressure-resistant sealed container, and 5 mL of acetonitrile was further added.The mixture was stirred at room temperature, and the reaction was checked by TLC, and the reaction was completed in 6 hours.The reaction solution was diluted with 10 mL of dichloromethane, and filtered to give a clear liquid.Separation by column chromatography (extraction of petroleum ether/ethyl acetate in a volume ratio of 50:1)The eluate containing the desired product were collected and the solvent was evaporated to give 4-iodo-benzonitrile as a white solid 52.7mg (46% yield).

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; Zhejiang University of Technology; Liu Yunkui; Zhang Jian; Bao Hanyang; (9 pag.)CN107641088; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com