Author: Jessica.F

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,
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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,
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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

Adding a certain compound to certain chemical reactions, such as: 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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 19094-56-5, HPLC of Formula: C7H4ClIO2

Oxalylchloride (176 kg; 1386 mol; 1.14 eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343 kg; 1214 mol) (compound IX.1), fluorobenzene (858 kg) and N,N-dimethylformamide (2 kg) within 3 hours at a temperature in the range from about 25 to 30 C. (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30 C. The solvent (291 kg) is distilled off at a temperature between 40 and 45 C. (p=200 mbar). Then the reaction solution (911 kg) is added to aluminiumchloride AlCl3 (181 kg) and fluorobenzene (192 kg) at a temperature between about 25 and 30 C. within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30 C. and stirred for an additional hour. After phase separation the organic phase (1200 kg) is separated into two halves (600 kg each). From the first half of the organic phase solvent (172 kg) is distilled off at a temperature of about 40 to 50 C. (p=200 mbar). Then 2-propanole (640 kg) is added. The solution is heated to about 50 C. and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1:4; 40 kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50 C. and p=200 mbar. Then 2-propanole (240 kg) is added at a temperature in the range between about 40 to 50 C. If the content of fluorobenzene is greater than 1% as determined via GC, another 140 kg of solvent are distilled off and 2-propanole (140 kg) is added. Then the solution is cooled from about 50 C. to 40 C. within one hour and seeding crystals (50 g) are added. The solution is further cooled from about 40 C. to 20 C. within 2 hours. Water (450 kg) is added at about 20 C. within 1 hour and the suspension is stirred at about 20 C. for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1:1; 800 kg). The product is dried until a water level of <0.06% w/w is obtained. The second half of the organic phase is processed identically. A total of 410 kg (94% yield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. 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-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see. Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/237526; (2011); A1;,
Iodide – Wikipedia,
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Electric Literature of 61272-76-2, 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. 61272-76-2, name is 4-Fluoro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 21 4-(((5-Fluoro-3-methyl-1H-indol-2-yl)methoxy)methyl)-N,N-dimethyl-1-phenylcyclohexanamine (one of two possible diastereomers) A mixture of Ain-12 (570 mg, 2 mmol), 4-fluoro-2-iodoaniline (Ian-04) (592 mg, 2.5 mmol), palladium(II) acetate (90 mg, 0.38 mmol), tetra-n-butylammonium chloride (564 mg, 2 mmol), triphenyl phosphine (203 mg, 0.80 mmol) and sodium carbonate (1.05 g, 10 mmol) was evacuated for 30 min in an oil pump. Anhydrous N,N-dimethyl formamide (15 ml), which had previously been flushed with argon for 1 h, was then added via a Schlenk attachment. The mixture was then stirred for 18 h at 100° C. The reaction mixture was then concentrated to small volume under vacuum. Toluene was repeatedly added to the residue, which was concentrated to small volume under vacuum each time and then divided between water and ethyl acetate (20 ml each). The phases were separated and the aqueous phase was extracted with ethyl acetate (3*30 ml). The combined organic phases were washed with 1 M sodium thiosultate solution (30 ml) and saturated sodium chloride solution (50 ml). The combined organic phases were dried with sodium sulfate and concentrated to small volume under vacuum. The crude product (1.06 g) was purified by MPLC [230 g, 46*3.6 cm, LiChroprep Si60 (15-25 mum)] with ethyl acetate/methanol (9:1). Yield: 319 mg (40percent), brown oil 1H-NMR (DMSO-d6): 1.25-1.70 (m, 7H); 1.90 (s, 6H); 2.21 (s, 3H); 2.56 (br d, 2H, J=11.9 Hz); 3.30 (d, 2H, J=6.3 Hz); 4.55 (s, 2H); 6.88 (ddd, 1H, J=9.5, 8.9, 2.6 Hz); 7.16-7.36 (m, 3H); 7.51-7.68 (m, 4H); 10.93 (s, 1H). 13C-NMR (DMSO-d6): 8.2; 24.4; 32.0; 36.9; 37.4; 58.5; 63.3; 74.8; 102.8 (d, J=23 Hz); 108.1; 109.0 (d, J=26 Hz); 111.8 (d, J=10 Hz); 126.1; 126.5; 127.2; 128.6 (d, J=12 Hz); 131.4; 131.9; 132.1; 132.2; 133.2; 133.9; 139.3; 156.5 (d, J=231 Hz).

The synthetic route of 4-Fluoro-2-iodoaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GRUNENTHAL GMBH; US2009/215725; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

68507-19-7, name is 3-Iodo-4-methoxybenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. category: iodides-buliding-blocks

3-iodo-4-methoxybenzoic acid (1.00 g, 7.19 mmol) was dissolved in SOCl2 (12.0 mL) and stirred at 80 C (22 h). Next, SOCl2 was removed in vacuo and azeotroped twice with benzene to give 57 (0.700 g, 2.36 mmol, 32%) as a white solid. 1H-NMR (400 MHz) CDC13: 8.50 (s, 1 H), 8.12-8.10 (d, 1 H), 6.88-6.86 (d, 1 H), 3.99 (s, 3 H); ,3C-NMR (100 MHz) CDC13: 165.1, 162.8, 141.9, 133.2, 126.3, 109.4, 85.2, 56.2.

The synthetic route of 68507-19-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; J-PHARMA CO., LTD.; WEMPE, Michael, F.; ENDOU, Hitoshi; WO2012/48058; (2012); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, 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 401-81-0, Safety of 1-Iodo-3-(trifluoromethyl)benzene

Dioxane (100 mL) was purged with nitrogen gas for 10 min. Phenanthrolene ( 1.0 g) and copper (I) iodide (1.0 g) were added to the dioxane, the suspension was allowed to stir under a nitrogen atmosphere for 5 min, and then cesium carbonate ( 18.72 g, 57.45 mmol), dimethyl malonate (5.46 g, 50.6 mmol), and l-iodo-3-(trifluoromethyl)benzene (12.5 g, 46.0 mmol) were added. The reaction mixture was heated to reflux for 18 h and then cooled to room temperature. Aqueous 1 N HC1 was added to the reaction mixture, the layers were separated, and the aqueous layer was extracted with ethyl acetate (3 x 100 mL). The combined organic layers were dried over magnesium sulfate and filtered. Celite diatomaceous filter aid (5 g) was added to the filtrate, and the resulting suspension was concentrated under reduced pressure at 50 C to yield a solid consisting of the crude product adsorbed onto Celite. This solid was purified by silica gel chromatography eluting with a gradient of 100% hexanes to 25% ethyl acetate in hexanes to yield 7.36 g (58.0%) of the title product. NMR (CDC13) delta 7.59-7.65 (m, 3H), 7.49 (t, 1H), 4.70 (s, 1H), 3.76 (s, 6H).

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-Iodo-3-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; ZHANG, Wenming; ANNIS, Gary David; WO2013/90547; (2013); A1;,
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. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 1,4-Diiodobutane

Stage 1 (0244) An oven-dried 3 L 4-neck flask fitted with an internal thermometer, N2 bubbler, overhead stirrer and oven-dried mL pressure-equalising dropping funnel was charged with 1,4-dibromo-2,5-diethylbenzene (70 g, 240 mmol) and dry THF (700 mL). The solution was cooled with stirring to <-70 C. to produce a white slurry. s-Butyllithium (335 mL, 1.4 M, 465 mmol) was charged to the dropping funnel and added dropwise over the space of 1.5 h ensuring the reaction temperature did not exceed -70 C. The slurry was stirred for 3 h after which GCMS confirmed the lithiation was complete. The dropping funnel was charged with a solution of 1,4-diiodobutane (13.8 mL, 105 mmol) in dry THF (140 mL) which was then added dropwise over 0.75 h. The resulting slurry was allowed to warm to room temperature and stirred for 12 h. The reaction was quenched by addition of water. The mixture was transferred to a separating funnel and the layers were separated. The aqueous layer was extracted with diethyl ether and the combined organics were washed with water, dried with MgSO4, filtered and concentrated to yield an orange oil. The product was triturated with 500 mL methanol for 0.5 h and filtered as a white solid before being recrystallised from toluene/IPA to yield a white powder that was dried in the oven (24.21 g, 48%). GCMS indicated a purity of 96% and the material was taken to the next stage without further purification The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Cambridge Display Technology Limited; Sumitomo Chemical Company Limited; Kamtekar, Kiran; Steudel, Annette; (30 pag.)US9812644; (2017); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, 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 31827-94-8, name: 2-Bromo-1-(4-iodophenyl)ethanone

General procedure: Sodium sulfite, sodium bicarbonate and sulfonyl chlorides in water were irradiated at 500 W for 20 min in a microwave oven. An ethanolic solution of the corresponding acetophenone was then added to sodium sulfinate and the reaction mixture was irradiated for 10 min to produce sulfones in good yields (1-13) (Scheme 2).

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; Paloque, Lucie; Bouhlel, Ahlem; Curti, Christophe; Dumtre, Aurelien; Verhaeghe, Pierre; Azas, Nadine; Vanelle, Patrice; European Journal of Medicinal Chemistry; vol. 46; 7; (2011); p. 2984 – 2991;,
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. 620-05-3, name is (Iodomethyl)benzene, A new synthetic method of this compound is introduced below., Recommanded Product: 620-05-3

General procedure: In a flame-dried round-bottom flask, beta-amidoester (9) (1 mmol; 1 equiv) was taken in DMF (5 mL) at room temperature. To this reaction mixture KOt-Bu (1.2 mmol; 1.2 equiv) was added. After 5 minutes of stirring at same temperature alkyl halide (1.05 mmol; 1.05 equiv) was added and stirring was continued for 15 minutes. Upon completion of the alkylation (judged by TLC), it was diluted with 10 mL of EtOAc and quenched with water. The organic extracts were dried over anhydrous sodium sulphate and concentrated under vacuum. The crude product was purified by flash chromatography (hexane and EtOAc as eluents) to afford compounds 10.

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:
Article; Kumar, Nivesh; Ghosh, Santanu; Bhunia, Subhajit; Bisai, Alakesh; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 1153 – 1169;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com