Category: iodides-buliding-blocks

Electric Literature of 444-29-1, 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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Pd(OAc)2 (22.4 mg, 0.10 mmol, 0.1 equiv), Ph3P (57.6 mg, 0.22, 0.22 equiv), and Cs2CO3 (1.63 g, 5 mmol, 5 equiv) were added to a flamedried, sealable vial under argon. Dry, degassed MeCN or DMF (3 mL) was added and the yellow mixture was stirred under argon for approximately 5 min. Aryl iodide (1.00 mmol, 1 equiv), alkyl iodide (10.00 mmol, 10 equiv), and olefin (5.00 mmol, 5 equiv) were added successively to the reaction mixture under argon. The mixture was stirred for 5 min, then solid norbornene (470 mg, 5.00 mmol, 5 equiv) was added. After a final argon purge, the vial was capped and placed in an oil bath that had been preheated to 90 °C. After 4?10 h, the mixture was cooled to r.t. Reactions performed in MeCN were filtered over a short pad of Celite (eluting with CH2Cl2) and concentrated in vacuo. Reactions performed in DMF were diluted with EtOAc? hexanes (1:1) and washed with brine twice. After drying with MgSO4, the organic layer was filtered and concentrated. The crude products were purified by flash column chromatography (CH2Cl2?hexanes, 1:5, then Et2O?hexanes, 1:100?1:25).

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-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 6828-35-9, The chemical industry reduces the impact on the environment during synthesis 6828-35-9, name is 5-Chloro-2-iodoaniline, I believe this compound will play a more active role in future production and life.

3-phenyl-2,2-dihydroxy-3-oxopropionic acid ethyl ester (0.05 mmol) was added to the reaction flask.2-iodo-5-chloroaniline (0.05 mmol),1,3-cyclohexanedione (0.05mmol),(R)-3,3,3′,3′-tetramethylspirophosphoric acid (0.005 mmol) represented by the formula (V),Anhydrous Na2SO4 (200mg),Inject 1 mL of dichloromethane and react at 65 C for 16 hours.After completion of the reaction, the residue was directly applied to silica gel column chromatography eluting with ethyl acetate / petroleum ether = 1:30 to give the corresponding optically active 1-arylindole derivative (I-4), yield 73% ;

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, 5-Chloro-2-iodoaniline, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 619-58-9, The chemical industry reduces the impact on the environment during synthesis 619-58-9, name is 4-Iodobenzoic acid, I believe this compound will play a more active role in future production and life.

A flame dried, 300-ml three-necked, round-bottomed flask equipped with a magnetic stirring bar was charged with 4-iodobenzoic acid 9 (10.0 g, 40.3 mmol) and THF (20.0 mL). To the solution were slowly added BH3·THF (1.06 M solution in THF, 60.0 mL, 63.6 mmol) at -20 C. After stirring for 12 h at 50 C, an additional portion of BH3·THF (1.06 M solution in THF, 60.0 mL, 63.6 mmol) was added at -20 C and the reaction mixture was refluxed for 2 h. The reaction was quenched with ice-H2O (100 mL) and K2CO3. The reaction mixture was concentrated under reduced pressure and the residue was extracted with EtOAc. The combined organic extracts were washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified on a short pad of silica gel (Hexanes/EtOAc, 10:1) to give the titled alcohol S-1 (9.90 g, quant) as a white solid. Its spectral data were identical with those reported1 ; IR (KBr) 3500-3000, 1483, 1400, 1005, 791 cm-1; 1H NMR (500 MHz, CDCl3) d 7.66 (2H, d, J = 8.0 Hz), 7.07 (2H, d, J = 8.0 Hz), 4.59 (2H, s), 2.11 (1H, s); 13C NMR (125 MHz, CDCl3) d 140.4, 137.5, 128.7, 92.9, 64.5.

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-Iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, A new synthetic method of this compound is introduced below., Formula: C8H4F13I

Reactions were conducted in a manner similar to Example 1 using the catalysts of the above Preparation Examples 2 to 4. The results of analysis are shown in the table below.

The synthetic route of 2043-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daikin Industries, Ltd.; US6664430; (2003); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 51839-15-7, 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. 51839-15-7, name is Dimethyl 5-iodoisophthalate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4.10 g (12.8 mmol) dimethyl 5-iodo-isophthalate were dissolved in 80 ml DMF. 3.32 g (20.1 mmol) 2-carbamoyl-phenylboric acid, 3.00 ml (21.6 mmol) TEA, 3.00 ml (167 mmol) water, 75 mg (0.33 mmol) palladium(II)-acetate as well as 102 mg (0.34 mmol) tri-ortho-tolylphosphine were added and the solution was heated to 100 C. for 2.5 h. The reaction solution was cooled and the solvent was distilled off i. vac. The residue was chromatographed on silica gel (gradient: DCM auf DCM/MeOH 7:3). 2.53 g (63%) of 11-a were obtained.RT (HPLC-MS)=2.68 min.ES-MS (M+H)+=314

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, Dimethyl 5-iodoisophthalate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Fuchs, Klaus; Eickmeier, Christian; Heine, Niklas; Peters, Stefan; Dorner-Ciossek, Cornelia; Handschuh, Sandra; Nar, Herbert; Klinder, Klaus; US2010/144681; (2010); 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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, A new synthetic method of this compound is introduced below., Formula: C7H6BrIO

To a solution of 2-bromo-5-iodoanisole (12.5 g, 40 mmol) in DCM (200 mL) was added a 1.0 M DCM solution OfBBr3 (40 mL) dropwise at 0 0C. The reaction mixture was then allowed to warm to room temperature. After stirring overnight, the reaction mixture was cooled to 0 C and MeOH (5 mL) was added dropwise. After stirring for 10 minutes at room temperature, the reaction mixture was washed with IN HCl (2 x 50 mL), water (50 mL) and brine (50 mL). The organic layer was dried over MgSO4. filtered and concentrated under vacuum. The residue was then dissolved in DMF (100 mL) and Cs2CO3 (26 g, 80 mmol) and 2-(benzyloxycarbonylamino)ethyl methanesulfonate (11 g, 40 mmol) were added. After stirring at 80C under nitrogen for 4 h, the reaction mixture was dissolved in EtOAc (100 mL). The organic layer was washed with brine (3 x 50 mL), dried over MgSO4 and filtered. The solvent was removed under vacuum and the crude compound was purified by flash chromatography using cyclohexane/EtOAc (85/15) as eluent to afford the title compound (11.5 g, 60% yield) as a white solid. ESMS; m/z 476, 478 (M+l), 493, 495 (M+18) 1H-NMR (CDCl3): 53.64 (q, J= 5.2 Hz, 2H), 4.05 (t, J= 4.7 Hz, 2H), 5.12 (s, 2H), 5.33 (bs, IH), 7.15-7.24 (m, 3H), 7.35 (bs, 5H).13C-NMR (CDCl3): 540.4, 67.0, 68.7, 92.4, 112.4, 122.7, 128.2, 128.2, 128.6, 131.5, 134.6, 136.4, 155.4, 156.4.Theoretical Mass: (M + Na) 497.91777. Measured Mass: (M + Na) 497.91638 Microanalysis: %C 40.41 (40.36), %H 3.24 (3.18), %N 2.86 (2.94) M.p. 700C

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; UCL BUSINESS PLC; WO2009/27679; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 1878-69-9, 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. 1878-69-9, name is 2-(3-Iodophenyl)acetic acid, This compound has unique chemical properties. The synthetic route is as follows.

200 mg (0.73 mmol) of (3-iodophenyl)acetic acid were dissolved in 4 mL of N,N dimethylacetamide and 244 mg (0.76 mmol) of TBTU, followed by 150 mu (o.80 mmol) of N-diisopropyl-N’-ethyl amine and 177 mg (1.1 mmol) of 3- (trifluoromethyl)aniline were added. The mixture was maintained at room temperature for 2 hours, then diluted withethylacetate, washed with aqueous NaHC03, HQ 2N, water and brine. The crude was triturated with a mixture diisopropyl ether-hexane affording, after filteration, 200 mg of the title compound as a white solid (68%). 1H NMR (401 MHz, DMSO-de) delta ppm 7.14 (t, J=7.75 Hz, 1 H) 7.35 (d, J=7.69 Hz, 1 H) 7.40 (d, J=7.81 Hz, 1 H) 7.55 (t, J=7.99 Hz, 1 H) 7.63 (dt, J=7.84, 1.39 Hz, 1 H) 7.73 (t, J=1.59 Hz, 1 H) 7.77 (d, J=8.30 Hz, 1 H) 8.08 (s, 1 H) 10.50 (s, 1 H)

The chemical industry reduces the impact on the environment during synthesis 2-(3-Iodophenyl)acetic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; NERVIANO MEDICAL SCIENCES S.R.L.; ANGIOLINI, Mauro; BUFFA, Laura; MENICHINCHERI, Maria; MOTTO, Ilaria; POLUCCI, Paolo; TRAQUANDI, Gabriella; ZUCCOTTO, Fabio; WO2014/184069; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 620621-48-9, 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 620621-48-9 as follows.

1. Synthetic routeAmong them, the condition (c) is LiBH4, toluene, 100 to 105 C, 30 to 35 min.2, the synthesis step(1) The purified intermediate compound C (C1, C2, C3) (0.5 g, 1.51 mmol, 1.51 mmol, 1.69 mmol) was weighed, and nitrogen gas was used as a protective gas. After adding 20 mL of toluene solvent, lithium borohydride (1.81 mmol, 1.81 mmol, 2.03 mmol) was added and reacted in an oil bath at 100-105 C for 30-35 min. The reaction endpoint was detected by TLC [developing agent: V (petroleum ether) / V (ethyl acetate) = 6 / 1];(2) After the reaction is completed, Slowly add 4M HCl solution under magnetic stirring to adjust the pH value of the system to 3~4.Add 50mL of deionized water, It was directly extracted with three portions of ethyl acetate and dried over anhydrous MgSO4. Then, it is filtered and concentrated to obtain a crude product of the compound intermediate D(D1,D2,D3). Purified by silica gel column chromatography [eluent: V ( petroleum ether) / V (ethyl acetate) = 12 / 1] The compound intermediate D(D1,D2,D3) is obtained, the white solids were 74%, 61% and 80%, respectively.

According to the analysis of related databases, 620621-48-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangdong University of Technology; Zhao Suqing; Zhang Bingjie; Feng Dongyan; Zhong Yingying; Huang Jinqu; Wu Ke; Ling Huaying; Tan Qiting; Chen Yanting; Zhao Jiawei; Ma Zhuolin; Jiang Zhengyun; Yang Yang; Zhu Qiuyan; Hong Weiqian; (37 pag.)CN110143869; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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. COA of Formula: C3H4F3I

General procedure: Example 20A Methyl 1-(2-methoxyethyl)-3,5-dimethyl-2,4-dioxo-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carboxylate 1.246 g (3.825 mmol) of caesium carbonate were added to a solution of 402 mg (1.25 mmol) of the compound from Ex. 18A in 12.3 ml of DMF, and the mixture was stirred at RT for 10 min. Then 452 mg (3.18 mmol) of iodomethane were added, and the mixture was stirred at RT for 22 h. The reaction mixture was then partitioned between water (75 ml) and dichloromethane (75 ml). The aqueous phase was extracted with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue obtained was chromatographed on silica gel (hexane/ethyl acetate eluent). 248 mg (59% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 4.47 (t, 2H), 4.14-4.06 (m, 4H), 3.65 (t, 2H), 3.24 (s, 3H), 2.86-2.73 (m, 5H), 2.65-2.54 (m, 2H) LC/MS (Method 3): Rt=1.39 min, m/z=477 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 460-37-7, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 877264-43-2, 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. 877264-43-2 name is (5-Fluoro-2-iodophenyl)methanol, 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.

To a solution of (5-fluoro-2-iodophenyl)methanol (3.78 g, 0.015 mol) in CH2CI2 (40 mL), imidazole (3.0 g, 0.045 mol) and TBDMS chloride (2.5 g, 0.016 mol) are added successfully, the reaction mass is stirred at room temperature for 8 hrs. After completion, reaction mass is quenched with water, washed with brine solution, extracted with CH2CI2, and the organic layer is dried over Na2S04, and concentrated to give tert-butyl((5-fluoro-2- iodobenzyl)oxy)dimethylsilane (3b) (Yield-88%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (5-Fluoro-2-iodophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; BIOPHORE INDIA PHARMACEUTICALS PVT. LTD.; PULLAGURLA, Manik Reddy; NANDA KUMAR, Mecheril Valsan; PITTA, Bhaskar Reddy; RANGISETTY, Jagadeesh Babu; (55 pag.)WO2017/183043; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com