Author: Jessica.F

Adding a certain compound to certain chemical reactions, such as: 2265-91-0, name is 1,3-Difluoro-5-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 2265-91-0, SDS of cas: 2265-91-0

8-methyl-6-phenyl-2H-[2,7]naphthyridine-l-one (200 mg, 0.846 mmol), CuI (32 mg, 0.169 mmol), K 3 PO 4 (359 mg, 1.692 mmol) were suspended in 1,4-dioxane (3 mL), dropwisely added with 3,5-difluoroiodobenzene(0.12 mL, 1.016 mmol), N,N – dimethylethylene diamine (0.036 mL, 0.338 mmol) and then refluxed for 15 hours under nitrogen atmosphere. The resultant was cooled down to room temperature, added with distilled water (50 mL) and then extracted with EtOAc (50 mL). The resulting organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate, filtered and concentrated. The resulting residue was purified by a silica gel column chromatograph (20% EtOAc/Etaexanes) and obtained a white solid [212 mg(72%)].[139] lambda Eta NMR(300 MHz, CDCl3) delta 3.16(s, 3H), 6.53(d, IH, J=7.2Hz), 6.88-6.95(m,IH), 6.98-7.06(m, 2H), 7. 27(d, IH, J=I. 2Hz), 7.43-7.55(m, 3H), 7.63(s, IH), 8.11-8.15(m, 2H).

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, 1,3-Difluoro-5-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SK CHEMICALS CO., LTD.; WO2006/112666; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 444-29-1, A common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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.

General procedure: A mixture of aryl halide (1.0 mmol), DAAD (1.1 mmol), and CuI (9 mg, 0.05 mmol) in DMF (2 mL) was stirred for 30 min at 0 °C. A suspension of NaH (0.050 g, 1.1 mmol) in DMF (1 mL) was slowly added to the reaction mixture over 20 min. The mixture was then evacuated and back-filled with N2 (3 times) and stirred for 12?20 h at the appropriate temperature. The crude reaction mixture was diluted with CH2Cl2 (5 mL) and a saturated NH4Cl solution (3 mL). The mixture was stirred for an additional 30 min and two layers were separated. The aqueous layer was extracted with CH2Cl2 (3 2 mL). The combined organic layers were dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexane/EtOAc 3:1) to give the desired product.

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Samzadeh-Kermani, Alireza; Tetrahedron Letters; vol. 57; 4; (2016); p. 463 – 465;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 181765-85-5 as follows. Formula: C8H6ClIO2

To a vial was added 1-005(221 mg, 0.506 mmol), methyl 4-chloro-2-iodobenzoate (150 mg, 0.506 mmol) and PdCl2(dppf CH2Cl2 (20.66 mg, 0.025 mmol). THF (3 mL) and 1.5 M Na2CO3 (1.012 mL, 1.518 mmol) were added. The mixture was bubbled with Ar for 3 min. The reaction mixture was sealed and irradiated in a microwave reactor at 100 C for 30 min. The reaction mixture was diluted with EtOAc and 0 and extracted with EtOAc. The combined organic layer was washed with brine, dried with MgS04 and concentrated. The crude residue was purified by ISCO (0-100% EtOAc in Hexanes) to afford the title compound (Example 313a, 160mg, 0.334 mmol, 66.0 % yield). MS (ESI) (m/z) 479 [M + H]+. FontWeight=”Bold” FontSize=”10″ H NMR (500 MHz, CDC13) delta 7.79 – 7.72 (m, 2H), 7.56 (dd, 7=8.0, 0.8 Hz, 1H), 7.38 (dd, 7=8.3, 2.2 Hz, 1H), 7.32 – 7.25 (m, 1H), 7.23 – 7.18 (m, 1H), 7.17 (d, 7=8.3 Hz, 2H), 7.02 (d, 7=8.3 Hz, 2H), 5.68 (s, 2H), 4.15 (q, 7=7.2 Hz, 2H), 3.79 (s, 3H), 3.57 (s, 3H), 1.52 (t, 7=7.0 Hz, 3H).

According to the analysis of related databases, 181765-85-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UNIVERSITE DE MONTREAL; BRISTOL-MYERS SQUIBB COMPANY; PRIESTLEY, Eldon, Scott; REZNIK, Samuel, Kaye; RUEDIGER, Edward, H.; GILLARD, James, R.; HALPERN, Oz, Scott; JIANG, Wen; RICHTER, Jeremy; RUEL, Rejean; TRIPATHY, Sasmita; YANG, Wu; ZHANG, Xiaojun; (642 pag.)WO2018/5591; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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