Category: 328-73-4

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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Iodo-3,5-bis(trifluoromethyl)benzene

Under a nitrogen atmosphere,Alpha-naphthol (7.2 g, 50 mmol),3,5-bis(trifluoromethyl)iodobenzene (20.4 g, 60 mmol),Barium carbonate (19.5 g, 60 mmol) was dissolved in 200 mL DMF.Additional palladium chloride (0.13 g, 0.75 mmol)As a catalyst,Heated at 115 ° C for 12 h,TLC monitors the progress of the reaction.The reaction is over,After falling to room temperature,Extracting the organic phase with ether,Dry over anhydrous MgSO4,filter,concentrate.Column chromatography gave the product as a dark brown oil.It was stirred and reacted with dihydropyran at room temperature for 10 h.A pale yellow solid k with a tetrahydropyran group is obtained.Under a nitrogen atmosphere,The intermediate product k (13.2 g, 30 mmol) was dissolved in 50 mLIn ether,The ice water bath is stable for 5 minutes.Add n-BuLi solution (14 mL, 33 mmol) dropwise.After 0.5 h of reaction, it gradually returned to room temperature.Continue to react for 4h,A large amount of white precipitate l was obtained.6.5 mL of diphenylphosphine chloride (PPh2Cl)Disperse evenly in 10 mL of ether,Under the ice water bath,Add dropwise to the original reaction system,Slowly rise to room temperature,The reaction was stirred overnight.TLC monitoring until the end of the reaction,Quenched with water,Extracting the organic phase with ether,The resulting organic phase was concentrated to 100 mL.Deaeration in the refrigeration cycle,Add 5 mL of concentrated hydrochloric acid under a nitrogen atmosphere.Reaction 5h,The reaction was followed by TLC.Neutralized by adding NaHCO3 aqueous solution,Quenched with water,Extracting the organic phase with ether,Dry over anhydrous MgSO4,filter,concentrate,Flash column chromatography gave 8.1 g of a white solid.The yield was 50percent.

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 328-73-4.

Reference:
Patent; Tianjin University; Li Yuesheng; Wang Xuling; Zhang Yanping; Pan Li; (25 pag.)CN109320558; (2019); A;,
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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

To a degassed solution of 1-iodo-3,5-bis(trifluoromethylbenzene (10.0 g, 29.4 mmol), anilinium hypophosphite (5.62 g, 35.3 mmol) and 3-aminopropyl triethoxysilane (7.81 g, 35.3 mmol) in anhydrous acetonitrile (200 mL) were added palladium acetate (132 mg, 0.588 mmol, 2 mol percent) and 1,3-bis(diphenylphosphino)propane (267 mg, 0.647 mol, 2.2 mol percent). The mixture was refluxed overnight. After cooling down to room temperature, the reaction mixture was diluted with ethyl acetate and hydrochloric acid (1M), and then partitioned. The aqueous layer was further extracted with ethyl acetate. The combined extracts were washed sequentially with aqueous sodium hydrogen carbonate and brine, and dried over sodium sulfate. The volatiles were removed in vacuo, and the residue was purified by column chromatography using 30 to 70percent ethyl acetate in petroleum ether to afford compound AZ3 (4.65 g) as a cloudy oil in 52percent yield. 1H NMR (CDCl3, 400 MHz): delta (ppm) 1.45 (t, J=7.1 Hz, 3H), 4.18-4.35 (m, 2H), 7.69 (d, J=579.6 Hz, 1H), 8.10 (s, 1H), 8.23 (s, 1H), 8.27 (s, 1H); 31P NMR (CDCl3, 161.8 MHz): delta (ppm) 19.59 (J=580.6 Hz).

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; Idenix Pharmaceuticals, Inc.; Parsy, Christophe Claude; Alexandre, Francois-Rene; Bonnaterre, Florence Marie-Emilie; Surleraux, Dominique; US9115095; (2015); B2;,
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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., name: 1-Iodo-3,5-bis(trifluoromethyl)benzene

General procedure: Sulfuric acid (400?800 muL) was added to a stirred mixture of iodoarene (1 mmol), Oxone (1 mmol, 617 mg) and arene (1.1?3 mmol) in acetonitrile (2 mL). The reaction mixture was stirred overnight and a solution of KBr (2 mmol, 240 mg) in water (10 mL) was added. After the formation of a solid or oily residue, acetonitrile was removed under reduced pressure. To the residue Et2O (10 mL) was added and the suspension stirred for 10 min. The precipitated diaryliodonium bromide was filtrated and washed with water (15 mL) and Et2O (15 mL). The product was dried under vacuo.

The synthetic route of 328-73-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Soldatova, Natalia; Postnikov, Pavel; Kukurina, Olga; Zhdankin, Viktor V.; Yoshimura, Akira; Wirth, Thomas; Yusubov, Mekhman S.; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 849 – 855;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 328-73-4, The chemical industry reduces the impact on the environment during synthesis 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

To a solution of compound 13a (125 mg, 0.412 mmol), and Et3N (1 mL) in DMF (4 mL), 1-iodo-3,5-bis(trifluoromethyl)benzene (146 muL, 0.824 mmol), CuI (15.7 mg, 0.082 mmol) and Pd(PPh3)4 (47.7 mg, 0.041 mmol) were added. The reaction mixture was stirred at room temperature overnight and filtered through a SiO2 pad. The residue was washed with 50percent EtOAc/hexane (4.x.15 mL) and concentrated in vacuo. The residue was purified by flash chromatography using 10percent EtOAc in hexane to afford 11a (138 mg, 65percent yield) as white solid. Rf (20percent EtOAc in hexane) 0.71; 1H NMR (300 MHz, CDCl3) delta 7.89 (s, 2H), 7.82 (s, 1H), 7.54-7.51 (m, 2H), 7.45-7.40 (m, 2H), 5.57 (s, 1H), 5.39 (br s, 1H), 4.55 (d, J=11.3 Hz, 2H), 4.11 (d, J=11.5 Hz, 2H), 1.50 (s, 9H); 13C NMR (75 MHz, CDCl3) delta 154.3, 137.1, 131.9, 129.4, 128.4, 128.4, 126.0, 124.6, 122.1, 102.0, 88.3, 82.9, 80.5, 72.8, 47.9, 28.4; IR (CH2Cl2): 3702, 3669, 3602, 3426, 2983, 2923, 2869, 1720, 1606, 1491, 1457, 1385, 1372, 1181, 1142; LRMS (EI): m/z 496 ([M+-F], 2), 459 (3), 430 (2), 399 (1); HRMS (EI): m/z calcd for C25H23NO4F5 [M+-F]: 496.1544, found: 496.1547.

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-3,5-bis(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ko, Rebecca Y. Y.; Chu, John C. K.; Chiu, Pauline; Tetrahedron; vol. 67; 14; (2011); p. 2542 – 2547;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 328-73-4, 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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The ligand L2 prepared in Example 4 was used as a reactant, 3,5-bistrifluoromethyliodobenzene, cuprous iodide, N,N’-dimethyl-1,2-ring in a xylene solvent. The hexamethylenediamine and potassium phosphate were reacted at a molar ratio of 1:2.0:0.2:0.4:2.0 at 90 °C for 6 hours, cooled to room temperature, diluted with ethyl acetate, filtered, concentrated, and obtained by column chromatography. The solid, ie the ligand shown by L4 (77percent yield), the specific synthetic route is as follows:

The synthetic route of 1-Iodo-3,5-bis(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shang Gu Science And Technology (Tianjin) Co., Ltd.; Wang Xiaomin; (35 pag.)CN108774216; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3F6I, 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. HPLC of Formula: C8H3F6I

General procedure: Arene (0.10 mmol, 1.0 equiv), Pd(OAc)2 (2.2 mg, 10 mumol,10 molpercent), ligand (15 molpercent or 20 molpercent), hydrogen phosphate (15 molpercent for benzylamine substrate), aryl iodide (0.3 mmol, 3.0 equiv.) and silver acetate (50 mg, 0.30 mmol, 3.0 equiv.) were added into a 2-dram reaction vial. Solvent and (+)-NBE-CO2Me (20 molpercent or 50 molpercent) were added to the mixture. The vial was flushed with N2 and capped. The reaction mixture was then stirred at the selected temperature for 12?24 h. After cooling to room temperature, the mixture was filtered through Celite and eluted with ethyl acetate. The filtrate was evaporated under reduced pressure. Purification by preparative thin-layer chromatography afforded the desired product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 328-73-4, its application will become more common.

Reference of 328-73-4,Some common heterocyclic compound, 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3F6I, 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: In a glovebox, aryl iodide (1.0 mmol), CsF (228 mg, 1.5 mmol), CuI (19.0 mg, 0.10 mmol), and PN-1 ligand (30 mg, 0.10 mmol) were weighed into a 4-dram borosilicate scintillation vial and dissolved in DMF (5 mL). Aryltriethoxysilane (1.0 mmol) was then added to the mixture, and the vial was tightly capped with a poly-seal conelined urea cap (Wheaton). The mixture was taken out of the glove box and placed in an oil bath pre-heated to 120 °C with vigorous stirring. After 48 h, the mixture was cooled to r.t., diluted with EtOAc (15 mL) and washed with H2O (3 × 5 mL). The aqueous fraction was back-extracted with EtOAc (3 × 5 mL). The combined organic fractions were dried (Na2SO4) and cotton-filtered, and the solvent was removed on a rotary evaporator. The product was purified by column chromatography (silica gel, hexanes, hexanes?Et2O, or hexanes?EtOAc).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Iodo-3,5-bis(trifluoromethyl)benzene, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 328-73-4, name is 1-Iodo-3,5-bis(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 328-73-4, name: 1-Iodo-3,5-bis(trifluoromethyl)benzene

EXAMPLE 7 Preparation of 2-(3,5-bis-(trifluoromethyl)-phenyl)-indene 20 ml of triethylamine, 2.2 g (20 mmole) of indene, 6.8 g (20 mmole) of 1-iodo-3,5-bis(trifluoromethyl)-benzene and 0.134 g (0.6 mmole) and 0.134 g (0.6 mmole) of Pd(OAc)2 were stirred under relux for 12 h. After it all triethylamine was removed under reduced pressure. The residue was treated with the mixture 50 ml of water and 50 ml of diethyl ether. Etherial layer was separated, washed twice with water, filtered and dried over Na2SO4. Ether was removed and some 20 ml of pentane were added to the reaction mixture, it was cooled down to -20¡ã C. and product was crystallized as dark needle crystals, which were filtered, washed with small portion of cold pentane and dried in vacuum. The yield of product was 32percent. 1H NMR (CDCl3): 8.06 (bs, 2H); 7.80 (bs, 1H); 7.58-7.48 (m, 3H); 7.42-7.32 (m, 2H); 3.88 (s, 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-Iodo-3,5-bis(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Montell Technology Company bv; US6271411; (2001); B1;,
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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C8H3F6I

General procedure: A typical procedure for the cross-coupling reaction using the nanocrystals is as follows: degassed N,N’-dimethylacetamide (DMA) (1.0 mL), aryl halide (0.5 mmol), trimethoxyphenylsilane (1.5 mmol), KF (1.5 mmol), tetrabutylammonium iodide (TBAI) (0.1 mmol), and Pd?Fe3O4 catalyst (1 molpercent) were added to a vial, which was equipped with a magnetic bar and purged with argon gas. The vial was sealed and the reaction mixture was heated to 150 ¡ãC for 16 h with vigorous stirring. After the reaction, the mixture was cooled to room temperature and the catalyst was collected using an external magnet. The solution containing products was diluted and extracted between dichloromethane (10 mL) and H2O(10 mL). The organic layer was dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by silica-gel column chromatography using a 1:6 mixture of ethyl acetate and n-hexane as an eluent to furnish the desired products.

According to the analysis of related databases, 328-73-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Lee, Woong-Sup; Byun, Sangmoon; Kwon, Jungmin; Kim, B. Moon; Bulletin of the Korean Chemical Society; vol. 37; 12; (2016); p. 1992 – 1997;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 328-73-4,Some common heterocyclic compound, 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3F6I, 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 bisallene (1 equiv), aryl/heteroaryl iodide (2.4 equiv), nucleophile (2.4 equiv), Pd2(dba)3 (5 molpercent), TFP (tri-(2-furyl)phosphine) (20 mol percent) and K2CO3 (6 equiv) in MeCN (5 mL) was stirred and heated at 80¡ãC (oil bath temperature). The mixture was filtered through a filter paper and the K2CO3 precipitate washed with MeCN (5 mL). The solvent was removed under reduced pressure, the residue dissolved in CHCl3 and washed with H2O (1¡Á20 mL). The organic layer was dried (anhydrous MgSO4), filtered and the filtrate evaporated under reduced pressure. The residue was purified by flash chromatography. 4.2.4. 1,3-Bis[(2Z)-4-(8-fluoro-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indol-2-yl)-3-(1H-indol-5-yl)but-2-en-1-yl]pyrimidine-2,4(1H,3H)-dione (14d). Prepared by general procedure B and heating for 1h. The solvent was cooled to precipitate the cascade product, filtered and the precipitate washed with water to dissolve K2CO3. The product 14d (0.12 g, 58 percent) crystallized from CHCl3 as pale yellow needles, mp 175?177¡ãC; deltaH (300 MHz, DMSO-d6); 11.06 (1H, br s, NH), 10.01 (1H, br s, NH), 10.86 (1H, s, NH), 10.84 (1H, s, NH), 7.80 (1H, d, J 7.9, pyrimidinyl?H), 7.70 (1H, s, Ar?H), 7.64 (1H, s, Ar?H), 7.32?7.18 (8H, m, Ar?H), 7.08 (1H, t, J 2.8, Ar?H), 7.05 (1H, t, J 2.6, Ar?H), 6.79 (2H, br t, J 9.2, Ar?H), 6.36 (2H, br s, Ar?H), 5.96 (1H, t, J 6.4, NCH2CH=), 5.79 (1H, t, J 6.5, NCH2CH=), 5.70 (1H, d, J 7.2, pyrimidinyl?H), 4.75 (2H, d, J 7.2, NCH2CH=), 4.72 (2H, d, J 7.2, NCH2CH=), 3.78 (4H, s, 2¡Á =CCH2N), 3.63 (4H, s, 2¡Á pyridoindolyl?CH2), 2.83 (4H, br s, 2¡Á pyridoindolyl?CH2), 2.69 (4H, br s, 2¡Á pyridoindolyl?CH2); numax/cm?1 (film); 3406, 1697, 1649, 1453, 1391, 1323, 1231; m/z (ESI+) 827.4 (100percent, MH+); (found MH+, 827.3640. C50H45F2N8O2 requires 827.3628).

The synthetic route of 328-73-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Elboray, Elghareeb E.; Aly, Moustafa F.; Abbas-Temirek, Hussien H.; Churchill, Gwydion H.; Grigg, Ronald; Tetrahedron; vol. 70; 1; (2014); p. 110 – 122;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com