Month: July 2021

Electric Literature of 629-09-4, A common heterocyclic compound, 629-09-4, name is 1,6-Diiodohexane, molecular formula is C6H12I2, 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.

Step-1 : Synthesis of 2-(6-iodohexyl)isoindoline-l,3-dione (3377) [1175] To a suspension of potassium phthalamide (700 mg, 3.7 mmol) in DMF (30 mL) was added 1 ,6-diiodohexane (3.83 g, 11.33 mmol) and the reaction mass was heated atw 80 C for 1 h. (The reaction mass became clear on heating). The reaction mixture was cooled to RT, diluted with diethyl ether (100 mL) and water (100 mL), the organic layers were separated, and the aqueous layer was again extracted with diethyl ether (2×100 mL). The combined organic layer was washed with water (200 mL) and saturated brine solution (200 mL) The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain the product, which was purified by column (3378) chromatography (silica gel: 100-200 mesh; Eluent: 10 % ethyl acetate in hexane) to obtain pure product as white solid (2.1 g).

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; MEDIVATION TECHNOLOGIES, INC.; HUNG, David; CHAKRAVARTY, Sarvajit; RAI, Roopa; BERNALES, Sebastian; SATHE, Balaji Dashrath; URETA, Gonzalo; MCCULLAGH, Emma; WO2015/116707; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 103962-05-6,Some common heterocyclic compound, 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, molecular formula is C7H4F3IO, 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.

A mixture of 5-Bromo-4,6-dimethyl-pyridin-2-amine (2 g), Cesium carbonate (6.46 g), 4- Trifluoromethoxy iodobenzene (4.29 g), Palladium (II) acetate (0.22 g, 0.99 minol) and 4,5- Bis(diphenylphosphino)-9,9-dimethylxanthene (0.57 g) was taken up in Toleune (40 mL) and degassed with nitrogen gas and heated at 120 °C for 5 h. The reaction was diluted with Water (50 mL) and extracted with Ethyl acetate (2 X 30 mL) and the combined organic extracts were driedover anhydrous Sodium sulphate and evaporated under reduced pressure. The residue was subjected to Silica gel flash column chromatography eluting with a gradient of Ethyl acetate and Heptane to obtain the title compound as an off white solid (2.7 g, 75 percent). LCMS: Rt: 2.44 min; MS:mz = 363.2 (M+2) 1H NMR (300 MHz, CDCI3) 6 7.36 (d, J = 9.0 Hz, 2H), 7.24 (d, J = 8.8 Hz, 2H), 2.66 (5, 3H), 2.39 (5, 3H).

The synthetic route of 103962-05-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; SAMBASIVAN, Sunderraman; NARINE, Arun; CHAUDHURI, Rupsha; VALLINAYAGAM, Ramakrishnan; VYAS, Devendra; ADISECHAN, Ashokkumar; DATTA, Gopal Krishna; (196 pag.)WO2018/108671; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 54811-38-0, These common heterocyclic compound, 54811-38-0, name is 5-Iodo-2-methylbenzoic 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 553-[4-Methyl-3-[[(tricycIo[3.3.1.13)7]dec-l-ylmethyl)amino]carbonyl]phenyl]-2-pyridinecarboxylic acida) 5-Iodo-2-methyl-7V-(tricyclo[3.3.1.13>7]dec-l-ylmethyl)-benzamide5-Iodo-2-methyl-benzoic acid (3.0 g) was stirred in dichloromethane (40 mL) undernitrogen. Oxalyl chloride (5 mL) was added followed by JV.JV-dimethylfonnamide (1 drop).After 2 hours the volatiles were removed under vacuum and the residue was redissolved indichloromethane (40 mL). Tricyclo[3.3.1.13>7]decane-l-methanamine (2.23 mL) andtriethylamine (3.18 mL) were added and the mixture was stirred under nitrogen for 2 hours.2M aqueous hydrochloric acid was added, the layers were separated and the aqueousfraction was extracted twice with dichloromethane. The combined organics were washedwith water, brine, dried (MgSO/O, filtered and concentrated in vacua. Purification bytrituration with diethyl ether afforded the sub-title compound (4.7 g).MS: APCI(+ve) 410 (M+H4).

The synthetic route of 54811-38-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2006/25783; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

17024-12-3, name is 9-Iodophenanthrene, 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. Recommanded Product: 17024-12-3

Synthesis of 1-[5-(1 ,1 ,3,3-tetramethylisoindolin-2-yloxylyl)-2-[9-(phenanthryl)]acetylene; 205 2079-lodophenanthrene (59 mg, 0.194 mmol), DABCO (62.5 mg, 0.557 mmol, 3 equiv) and Pd(OAc)2 (1 mg, 2.5 mol %) was dissolved in dry MeCN (1 cm3). 5-ethynyl- 1,1,3,3-tetramethylisoindolin-2-yloxyl 205 (50 mg, 0.233 mmol, 1.2 equiv) was added and mixture heated at 80 0C under argon for 4 h. Subsequently the solvent was removed under reduced pressure and the residue taken up in CHCI3 (~1 ml) ensuring the DABCO remained undissolved. Purification of the resulting solution by column chromatography (SiO2, eluant:10 % EtOAc, 90 % n-Hexane) gave 1 -[5-(1 , 1,3,3- tetramethylisoindolin-2-yloxylyl)-2-[9-(phenanthryl)]acetylene, 207 (68 mg, 0.175 mmol, 90 %).

The synthetic route of 17024-12-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; QUEENSLAND UNIVERSITY OF TECHNOLOGY; WO2007/124543; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 60577-34-6,Some common heterocyclic compound, 60577-34-6, name is 4-Iodo-N-methylaniline, molecular formula is C7H8IN, 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.

46.6 mg (0.2 mmol) of N-methyl 4-iodoaniline, 81.2 mg of ethyl bromodifluoroacetate (0.4 mmol), 2.5 mg (0.02 mmol) of cuprous acetate, 19.1 mg (0.04 mmol) of X-phos, 32.7 mg (0.2 mmol) of cesium carbonate were added to 2 mL of DMF solvent. The reaction was carried out at 110 C for 12 hours, after the reaction was completed, it was cooled, filtered, and the filtrate was evaporated. The solvent was removed and the residue was chromatographed on silica gel. It was washed with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 8:1. The effluent was collected according to the actual gradient, detected by TLC, and the effluent containing the product was combined. The solvent was distilled off by a rotary evaporator. Vacuum drying to give a yellow liquid N-(p-iodophenyl)-N-methylformamide 27.1 mg, yield 52%.

The synthetic route of 60577-34-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou University; Zhang Xiaohong; Li Xiaofang; Zhang Xingguo; (15 pag.)CN108774147; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 156150-67-3, The chemical industry reduces the impact on the environment during synthesis 156150-67-3, name is 2-Chloro-1-fluoro-4-iodobenzene, I believe this compound will play a more active role in future production and life.

2-chloro-1-fluoro-4-iodobenzene (771) mg) In the dioxane (5 mL) solution of tert-butyl 5-hydroxy-4-methyl-2,3-dihydro-1H-indole- 1-carboxylate (500 mg), and copper iodide (I) (38.2 mg), N,N-dimethylglycine (41.4 mg) and cesium carbonate (1.31 g) were added, and it stirred at 100 degrees C for 3 hours and 25 minutes. Cerite filtration of the reaction mixture was carried out after cooling to a room temperature. The mark compound (57.8 mg) was obtained as a colorless solid by condensing under decompression of the obtained filtrate and refining residue with silica gel column chromatography (ethyl acetate/hexane).

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-1-fluoro-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DAIICHI SANKYO COMPANY LIMITED; NAGAMOCHI, MASATOSHI; GOTANDA, KENTOKU; GOTO, TAIJI; SASAKI, JUNKO; YOSHINO, TOSHIHARU; ISOBE, TAKASHI; (75 pag.)JP2016/128387; (2016); A;,
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. 217314-45-9, name is Methyl 3-amino-5-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8H8INO2

Step C: Mesylation; To a 0 C solution of aniline from step B (21.7 g, 78.3 mmol) in 3:1 1 CH2Cl2: pyridine (75 mL) was added methanesulfonyl chloride (6.36 mL, 82.2 mmol). The ice bath was removed after 15 min and the solution was stirred overnight at rt. The reaction mixture was extracted several times with IN HCI. The organic phase was dried, concentrated, and chromatographed (1:1 EtOAc:Hex) to afford 25.2 g of the desired sulfonamide as a white solid.

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 217314-45-9.

Reference:
Patent; MERCK & CO., INC.; WO2005/103020; (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. 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, A new synthetic method of this compound is introduced below., Quality Control of (5-Bromo-2-iodophenyl)methanol

A solution of 9.59 mmol (5-bromo-2-iodo-phenyl)-methanol [199786-58-8] in 10 ml of N,N-dimethylformamide is added at room temperature dropwise to a mixture of 11.5 mmol of sodium hydride (60% in paraffine) in 20 ml of N,N-dimethylformamide. The mixture is stirred for 1 h at room temperature. 10.6 mmol of tert-butyl-dimethyl- chloro silane and 1.00 mmol of potassium iodide are added and the mixture stirred for 30 minutes at room temperature. The reaction is quenched with water and extracted with toluene. The combined organics are washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. , The resulting residue is purified by flash chromatography (SiO2 60F) to afford the title compound as colourless oil. Rf = 0.35 (dichloromethane); Rt = 11.31 (gradient II).

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; SPEEDEL EXPERIMENTA AG; WO2008/119744; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 1829-28-3, The chemical industry reduces the impact on the environment during synthesis 1829-28-3, name is Ethyl 2-iodobenzoate, I believe this compound will play a more active role in future production and life.

In a test tube equipped with a stirrer and a septum cap, trifluoromethylzinc iodide (DMPU) 2 complex (160 mg, 0.2 mmol) prepared in Example 1 and copper (I) iodide (1.9 mg, 0.01 mmol ) Was charged, and argon substitution was carried out three times. Then, a solution of ethyl 2-iodobenzoate (16.6 mul, 0.1 mmol) in DMPU (0.2 ml) was added, the septum cap was replaced with a screw chap, and the reaction was carried out at 50 ° C. for 24 hours. After completion of the reaction, the reaction solution was quantified with 19 F-NMR (benzotrifluoride internal standard), and ethyl 2-trifluoromethylbenzoate was produced with a yield of 80percent

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, Ethyl 2-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TOKYO INSTITUTE OF TECHNOLOGY; TOSOH F-TECH INCORPORATED; MIKAMI, MIKAMI; NAKAMURA, YUZO; NEGISHI, KAZUYUKI; AIKAWA, KOHSUKE; (8 pag.)JP5889817; (2016); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application 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 (45 mg; 0.2 mmol) and triphenylphosphine (115 mg; 0.44 mmol) were filled into anoven dried sealable tube and dissolved in dry MeCN (12 mL) under argon atmosphere. After5 min Cs2CO3 (3.26 g; 10 mmol), the aryl iodide (2 mmol), 1,3-dibromopropane (2.04 mL;20 mmol; for iodobenzene (1a): 2.24 mL; 22 mmol) and methylacrylate (906 muL; 10 mmol)were added. The reaction mixture was purged with argon for 5 min. After addition ofnorbornene (942 mg; 10 mmol) the tube was sealed and heated at 90 °C for 18 h.For workup the cooled reaction mixture was filtered over Celite®, washed with DCM,concentrated in vacuo and purified by column chromatography.

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.

Reference:
Article; Stark, Tina; Suhartono, Marcel; Goebel, Michael W.; Lautens, Mark; Synlett; vol. 24; 20; (2013); p. 2730 – 2734;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com