Iodides-buliding-blocks

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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, A new synthetic method of this compound is introduced below., name: Methyl 5-bromo-2-iodobenzoate

(a) 5-Bromo-2-(4-nitrobenzoyl)benzoic acid methyl ester; /-PrMgCI LiCI in THF (1.25M.17.6 ml_, 22 mmol) was added to 5-bromo-2-iodo- benzoic acid methyl ester (6.82 g, 20 mmol) in THF (40 ml_) at -40 0C over 5 min. The mixture was stirred at -30 0C for 1 h, cooled to -78 0C and added to 4-nitro- benzoyl chloride (7.42 g, 40 mmol) in THF (30 mL) at -78 0C. The temperature was allowed to reach rt and NaHCO3 (aq, sat) was added. Extractive workup (EtOAc, NaHCO3 (aq, sat), H2O, brine), drying (K2CO3 and Na2SO4), concentration and crystallization from EtOAc gave the sub-title compound. Yield: 5.48 g (75%).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOLIPOX AB; NILSSON, Peter; PELCMAN, Benjamin; KATKEVICS, Martins; WO2010/103279; (2010); A1;,
Iodide – Wikipedia,
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Application of 90347-66-3, These common heterocyclic compound, 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, 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.

Reference Example 1Methyl 3-ethynyl-4-methylbenzoateA mixture of methyl 3-iodo-4-methylbenzoate (2.0g, 7mmol), trimethylsilylacetylene (1.2ml, 8mmol), Pd(PPh3)4 (0.42g, 0.3mmol), Cul (0.137g, 0.7mmol) and diisopropylethylamine (2.5ml, 1 1.4mmol) in THF (20ml) was heated at 50C for 12hrs under nitrogen atmosphere. The reaction mixture was cooled to ambient temperature and filtered through a Celite bed. The clear filtrate was concentrated and the residue purified by flash chromatography on silica gel (elution with 2% ethyl acetate in n-hexane) to provide methyl 4-methyl-3-[(trimethylsilyl)ethynyl]benzoate.To the solution of methyl 4-methyl-3-[(trimethylsilyl)ethynyl]benzoate (2.3g) in THF (40ml) was added tetrabutylammonium fluoride (1.0M in THF, 3.2ml, 1 lmmol) at ambient temperature and stirred for 15 minutes, concentrated and the residue purified by flash chromatography on silica gel (elution with 2% ethyl acetate in ?-hexane) to provide methyl 3 – ethynyl- 4-methylbenzo at e .? NMR (500 MHz in DMSO-de), delta 2.50 (s, 3H), 3.90 (s, 3H), 4.57 (s, 1H), 7.51 (d, J = 8.0 Hz, 1H), 7.91 (d, J = 8.0 Hz, 1H), 7.99 (s, 1H).

The synthetic route of 90347-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUN PHARMA ADVANCED RESEARCH COMPANY LTD; SENGUPTA, Prabal; CHOKSHI, Hemant Ashvinbhai; PURI, Chetan Surjitsingh; CHIMANWALA, Sabbirhusen Yusufbhai; MEHTA, Varun Anilkumar; DESAI, Dipali Manubhai; CHITTURI, Trinadha Rao; THENNATI, Rajamannar; ATKINSON, Jonathan David Mark; WO2012/98416; (2012); A1;,
Iodide – Wikipedia,
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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. 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, A new synthetic method of this compound is introduced below., name: 2-Iodo-5-methylbenzoic acid

Step B: Methyl 2-iodo-5-methyl-benzoate The compound of the above Step (6.25 g, 23.9 mmol) is dissolved in anhydrous methanol (100 mL), and then SOCl2 (3.6 mL, 49 mmol) is added dropwise to the well-stirred solution. The solution is refluxed for 18 hours and then evaporated to a volume of 25 mL and then poured into crushed ice (100 g). The resulting mixture is extracted with diethyl ether (2*75 mL). The organic phase is washed with saturated aqueous NaHCO3 solution and then brine, dried over Na2SO4 and evaporated to dryness to yield the title compound.

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; LE TIRAN, Arnaud; LE DIGUARHER, Thierry; STARCK, Jerome-Benoit; HENLIN, Jean-Michel; GUILLOUZIC, Anne-Francoise; DE NANTEUIL, Guillaume; GENESTE, Olivier; FEJES, Imre; TATAI, Janos; NYERGES, Miklos; DAVIDSON, James Edward Paul; MURRAY, James Brooke; CHEN, I-Jen; DURAND, Didier; US2015/31673; (2015); A1;,
Iodide – Wikipedia,
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Related Products of 20555-91-3, These common heterocyclic compound, 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, 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: An efficacious one-pot synthesis method reported by Bielawskiet al. (2007) was adopted with minor modifications in this section. The overall route is shown in Scheme 2, andthe obtained compounds listed in Fig. 2. Briefly, to a 50-mL round-bottomed flask was added substituted iodobenzene(5 mmol), 20 mL of DCM, and mCPBA 1.22 g(6 mmol, 85% purity), followed by the slow addition of(2-(2-(2-methoxyethoxy)ethoxy)ethoxy)benzene 1.31 mL(6 mmol). After cooling the mixture to 0 C, trifluoromethanesulfonic acid 0.75 mL (8.5 mmol) was added dropwise into the system. The resulting solution wasstirred at room temperature for 2 h. The crude product was purified by column chromatography on silica gel eluted with a mixture of DCM:methanol (20:1, vol.) to yield the desired products.

Statistics shows that 1,2-Dichloro-4-iodobenzene is playing an increasingly important role. we look forward to future research findings about 20555-91-3.

Reference:
Article; Huang, Mengen; Xu, Shujia; Wu, Xunshen; Zhao, Min; Wang, Limin; Journal of Surfactants and Detergents; vol. 21; 3; (2018); p. 323 – 334;,
Iodide – Wikipedia,
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Application of 20555-91-3, The chemical industry reduces the impact on the environment during synthesis 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, I believe this compound will play a more active role in future production and life.

Method B: a mixture of 3,4-dichlorolodobenzene (300 mg), propargyl alcohol (128 mul_), CuI (10 mg), K2CO3 (302 mg), Pd(PPh3)4 (12 mg) in DMF (2 mL) was irradiated with MicroWave at 100 0C for 20 min. Aqueous saturated solution NH4CI was then added followed by DCM. After separation of the two phases the organic layer was dried and evaporated in vacuo. The crude product was purified by flash chromatography (eluting with cyclohexane / ethyl acetate 7/3) to give the title compound (40 mg). NMR (1H, CDCI3): delta 7.58 (s, 1 H), 7.41 (d, 1 H), 7.27 (d, 1 H), 4.52 (d, 2H), 1.75 (t, 1 H)

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, 1,2-Dichloro-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXO GROUP LIMITED; DI FABIO, Romano; MICHELI, Fabrizio; TEDESCO, Giovanna; TERRENI, Silvia; WO2008/31771; (2008); A2;,
Iodide – Wikipedia,
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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 64248-58-4 as follows. Application In Synthesis of 1,2-Difluoro-4-iodobenzene

a) (3,4-Difluoro-phenyl)-propynoic acid ethyl ester (Vc) Under argon atmosphere, a four neck flask was charged with THF (135 ml) and 2 M LDA in THF (60.9 ml, 0.12 mol, 1.18 eq.) and cooled to -78 C. Propynoic acid ethyl ester (12.2 g, 0.12 mol, 1.18 eq.) dissolved in THF (36 ml) was added dropwise within 30 min. Then, ZnBr2 (28.5 g, 0.12 mol, 1.2 eq.) dissolved in THF (45 ml) was added dropwise within 30 min. After the addition of 1,2-Difluoro-4-iodo-benzene (25.0 g, 0.10 mol) and tetrakis(triphenylphosphine) palladium(0) (6.02 g, 5.15 mmol, 5 mol %), the reaction mixture was allowed to warm to r.t. and stirred for another 3 h at the same temperature. The reaction mixture was diluted with diethylether and washed with saturated aqueous NH4I, saturated aqueous NaHCO3 and brine. The organic phase was dried with Na2SO4, concentrated under reduced pressure and dried under vacuum. The residue was purified by silica gel filtration (heptane/ethyl acetate 98:2) to yield 16.6 g (76%) of Vc as light yellow oil. ES-MS m/c: 210 (M+).

According to the analysis of related databases, 64248-58-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hoffmann-Emery, Fabienne; Puentener, Kurt; Ratni, Hasane; US2010/152462; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 181765-86-6,Some common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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.

2,9 g (14,9 mmol) of (1 , 1′-biphenyl)-2-yl-boronic acid, 4,6 g (13,6 mmol) of methyl 5-bromo-2-iodobenzoate, 314 mg (0,3 mmol, 0,02 eq.) of Pd(P(Ph3))4, 5,6 g (40,7mmol, 3 eq.) of Na2C03 are dissolved in 7 mL of water and 30 mL of toluene. The reaction mixture is stirred at 85C and agitated under an argon atmosphere for 12 hours and after cooling to room temperature, the mixture is filtered through Celite. The filtrate is evaporated in vacuo, and the residue is purified by (0273) chromatography (mixture heptane/AcOEt). The product is isolated in the form of an off-white solid (4,5 g 91 % of theory).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK PATENT GMBH; MONTENEGRO, Elvira; MUJICA-FERNAUD, Teresa; MAIER-FLAIG, Florian; VOGES, Frank; COMELY, Alexander; MORENO FLORES, Rosa; (201 pag.)WO2019/115577; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 811842-30-5, name is 2-Bromo-1-fluoro-4-iodobenzene, 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. Recommanded Product: 2-Bromo-1-fluoro-4-iodobenzene

Add 9H-purin-2-amine (135 mg, 1 mmol), 2-bromo-1-fluoro-4-iodobenzene (600 mg, 2 mmol), potassium carbonate (415 mg, 3 mmol) and proline(23 mg, 0.2 mmol) to the eggplant type flask, dimethyl sulfoxide was added, and the reaction solution was deoxidized. Copper iodide (19 mg, 0.1 mmol) was added and the reaction solution was deoxygenated. Heat to 90 C and stir for 16 hours. After the reaction was completed, it was cooled to room temperature, water and ethyl acetate were added, and the mixture was filtered over Celite.The target compound (QC87-1) 40 mg was obtained, ESI-MS calc. C11H779BrFN5[M+H]+= 307.99; experimentally measured: 307.39;the target compound (QC87-2) 40 mg was obtained.

The synthetic route of 2-Bromo-1-fluoro-4-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Shanghai Pharmaceutical Institute; Zhao Yujun; Li Zhiqiang; Yan Ziqin; Li Jia; Zhou Yubo; Su Mingbo; Chen Zheng; (138 pag.)CN109810110; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, name is 1,4-Diiodobutane, 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. HPLC of Formula: C4H8I2

Example 3 (n=4); (a) 1, 1′-[(Butane-1,4-diyl)dioxy]bis[(11S,11aS)-10-(tert- butyloxycarbonyl)-8-methoxy-ll- (tetrahydro-pyran-2-yloxy)- 1, 2,3, 10, 11, 11a-hexahydro-5H-pyrrolo[2,-c][1,4]benzodiazepine-5-one](8b); 1,4-Diiodobutane (69.1 mg, was added to the mixture of monomer 7 (0.2 g, 0.44 mmol, 1.0 equiv) and potassium carbonate (0.98 mmol, 2.2 equiv) in dry DMF (30 mL), and the resulting mixture was heated to 90C under a nitrogen atmosphere for 5 h. Removal of excess solvent under reduced pressure afforded a crude solid, which was subjected to flash column chromatography (SiO2, 50% EtOAc- hexane) to afford the dimerized compound 8b (134 mg, 0.14 mmol, 63% yield, mixture of diastereomers from THP protecting group as a solid: [a] 20D = +36 (c = 0. 19, CHCl3) ; 1H NMR (CDC, 400 MHz): 5 1.35 (s, 36H, Boc), 1.45-1. 67 (m, 16H, THP), 1.68-1. 86 (m, 8H, THP), 1.90-2. 21 (m, 24H, 1-H, 2-H, 13-H), 3.44-3. 78 (m, 16H, 3-H, lla-H, THP), 3.84-4. 02 (m, 16H, 7-OMe, THP), 4. 04-4. 25 (m, 8H, 12- H), 5.02-5. 10 (m, 2H, THP), 5.11-5. 20 (m, 2H, THP), 5.69-5. 77 (d, 2H, 11-H), 5.79-5. 89 (d, 2H, 11-H), 6.51 (s, 2H, 9-H), 6.88 (s, 2H, 9-H), 7.19 (s, 2H, 6-H), 7.28 (s, 2H, 6-H) ; 13C NMR (CDCl3, 400 MHz): No. 19.8, 20.5, 23.1, 23.2, 25.3, 25.9, 28.1, 28. 2,28. 9, 29.1, 30.9, 31.2, 46.2, 55.9, 56.2, 60.1, 63.3, 63.6, 68.6, 80.9, 88.2, 91.2, 96.2, 100.2, 111.1, 111.4, 113.4, 114.1, 118.5, 126.4, 129.8, 143.1, 147.9, 148.2, 151. 5, 151. 8,155. 8,167. 4,167. 6; IR (neat): 2945,1704, 1644, 1604,1513, 1449,1392, 1327,1217, 1163, 1022cm~1 ; MS (FAB) m/z (relative intensity) 973 ([M + Na] +, 11), 951 (M +, 100), 749 (36).

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SPIROGEN LIMITED; WO2005/85259; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 3032-81-3, 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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 1,3-dichloro-5-iodo-benzene in 1,4-dioxane (160 mL) was added Copper(I) iodide (0.661g), pyridine-2-carboxylic acid (0.812g), and cesium carbonate (32g) under Argon. Then dimethyl propanedioate (15g) was added at room temperature via dropping funnel.The mixture was heated to 90C for 5h. After completion of the reaction mixture was diluted with water and extracted with ethyl acetate (2x). the combinated organic layers were washed with brine, dried over sodium sulphate and concentrated. The crude was purified by silica gel column chromatography (3RF 200) using a gradient of ethyl acetate (0 to 10%) in cyclohexane to give the title compound (11.75 g, 77.1% Yield). LC-MS (method A): 277 (M+1)+, 275 (M-1)+retention time 1.02 min.

The synthetic route of 1,3-Dichloro-5-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; JUNG, Pierre, Joseph, Marcel; DUMEUNIER, Raphael; GAGNEPAIN, Julien, Daniel, Henri; STOLLER, Andre; RENDINE, Stefano; (165 pag.)WO2019/115404; (2019); A1;,
Iodide – Wikipedia,
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