Month: July 2021

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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 31599-61-8

General procedure: Aryl thiourea (1, 0.5 mmol), aryl iodide (2, 0.6 mmol), CuSO4*5H2O (0.05 mmol), Cs2CO3 (2.0 equiv), 2,2?-bypyridine (0.05 mmol) were added in sealed tube equipped with a septum and magnetic stirring bar, H2O (2.0 mL) was then added. The mixture was stirred at 100 C and checked by TLC until the starting material was finished (about 3h). The reaction was terminated with sat. NH4Cl solution (3 mL) and then extracted with ethyl acetate. The crude solution was dried over anhydrous Na2SO4 and evaporated under vacuum. The residue was purified by flash column chromatography to afford the desired product 3a.

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 31599-61-8.

Reference:
Article; Liu, Xing; Zhu, Hui; Zhang, Shi-Bo; Cheng, Yu; Peng, Han-Ying; Dong, Zhi-Bing; Tetrahedron Letters; vol. 59; 33; (2018); p. 3165 – 3170;,
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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, A new synthetic method of this compound is introduced below., Quality Control of 4-Iodo-1,2-dimethylbenzene

General procedure: A mixture containing styrene (3.5 mmol), aryl halide (3.5 mmol), the palladium complex [(L)PdCl] (0.001 mmol) and potassium carbonate (8.0 mmol) in methanol (10 ml) were heated to reflux for 4 h. After evaporation of solvent the product was poured into water and extracted with diethyl ether. The ether solution was dried over Na2SO4 and filtered. The ether solution were passed through silica column (60-120 mesh), the complex remain trapped. After extraction of desired compound complex was extracted using dichloromethane. Upon evaporation of the ether, solid of pure products were obtained. The yields of the products obtained from all the reactions were determined after isolation and characterized by 1H NMR spectra.

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:
Article; Pattanayak, Poulami; Pratihar, Jahar Lal; Patra, Debprasad; Lin, Chia-Her; Paul, Sobhana; Chakraborty, Kausiki; Polyhedron; vol. 51; 1; (2013); p. 275 – 282;,
Iodide – Wikipedia,
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Related Products of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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: To a 10 mL glass tube aryl halide (1 mmol), K4FeCN6(0.6 mmol,220 mg), K2CO3(1.5 mmol, 207 mg), catalyst (10 mg), and 2 mL DMFwere added and mixture was stirred for appropriate reaction timeat 120C under argon atmosphere. The progress of the reactionwas monitored by GC analysis. After completion of the reaction,reaction mixture was washed with 5 mL water and crude productwas isolated using dichloromethane (5× 1 mL). Organic extractswere combined together, evaporated and purified by flash chro-matography using hexane/EtOAc to give the desired aryl cyanideproducts.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Iodobenzaldehyde, its application will become more common.

Reference:
Article; Gholinejad, Mohammad; Aminianfar, Afsaneh; Journal of Molecular Catalysis A: Chemical; vol. 397; (2015); p. 99 – 105;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 69113-59-3, These common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, 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.

The title compound (40 mg, 66.4 %, white solid) was obtained from [4- [1- (5-] [TRIBUTYLSTANNANYL-ISOXAZOL-3-YL)-ETHYL]-PIPERAZINE-1-CARBOXYLIC] acid ethyl ester (109 mg, 0.2 mmol) and Pd (PPh3) [2C12] (2.0 mg) with 3-iodo-benzonitrile (45.7 mg, 0.17 mmol) in dioxane [(LUT)] at [110 C OVERNIGHT. LH-NMR (CDCL3) B] (ppm): [8.] 07 (s, 1H), 8.05 (d, 1H), 7.63 (d, 1H), 7.62 (t, [1H),] 6.62 (s, [1H),] 4.12 (q, 2H), 3.88 (q, [1H),] 3.50 (m, 4H), 2.52 (m, 4H), 1.47 (d, 3H) and 1.25 (t, 3H).

Statistics shows that 3-Iodobenzonitrile is playing an increasingly important role. we look forward to future research findings about 69113-59-3.

Reference:
Patent; ASTRAZENECA AB; NPS PHARMACEUTICALS, INC.; WO2004/14370; (2004); A2;,
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. 645-00-1, name is 1-Iodo-3-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 645-00-1

General procedure: A mixture of the aryl halide (0.5 mmol), phenylacetylene(0.5 mmol), piperidine (1 mmol), ortho-palladated catalyst(0.2 mol %) was added to NMP (3 mL) in round-bottom flask equipped with condenser and placed into the Milestone microwave. Initially using a microwave power of 600 W the temperature was ramped from room temperature to 100 C and then held at this temperature until the reaction was completed. During this time, the power was modulated automatically to keep the reaction mixture at 100 C. The mixture was stirred continuously during the reaction and monitored by both TLC and GC. After the reaction was complete, the mixture was cooled to room temperature and was diluted with n-hexane and water. The organic phase was dried over MgSO4, filtered and concentrated under reduced pressure using rotary evaporator. The residue was purified by silica gel column chromatography.

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 645-00-1.

Reference:
Article; Hajipour, Abdol R.; Rafiee, Fatemeh; Journal of the Iranian Chemical Society; vol. 12; 7; (2015); p. 1163 – 1169;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 624-75-9, name is 2-Iodoacetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C2H2IN

To a mixture of 5-bromo-2-isopropyl-4-methoxy-phenol from step 4 (0.831 g, 3.4 mmol) and K2CO3 (0.562 g, 4.1 mmol) in 17 mL dimethyl formamide (DMF) was added iodoacetonitrile (0.594 g, 3.6 mmol). The mixture was warmed to 60 C. for 30 minutes and then allowed to cool to room temperature. After cooling to room temperature the mixture was taken up in 50 mL of H2O and extracted with 1:1 toluene/ethyl acetate, washed with H2O and then with brine. The combined organic layers were dried over Na2SO4, filtered and conectrated in vacuo to give a crude solid. Purification via flash chromatography (1:1 hexane/CH2Cl2) afforded (5-bromo-2-isopropyl-4-methoxy-phenoxy)-acetonitrile (0.611 g, 63%) as a while solid.

The synthetic route of 624-75-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Roche Palo Alto LLC; US2005/209260; (2005); A1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, molecular formula is C8H8INO2, 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. Safety of Methyl 4-amino-3-iodobenzoate

A solution of 3.00 g (10.8 mmol) of methyl 4-amino-3-iodobenzoate and 1.30 g (54.1 mmol) of lithium hydroxide in 150 ml of a dioxane/water mixture (1:1) was stirred at room temperature for 6 h. The dioxane was distilled off in vacuo, and the remaining aqueous phase was adjusted to pH 5 with 1 M hydrochloric acid. The precipitate was filtered off with suction and washed with water. 2.80 g (98%) of the title compound were obtained as a solid. HPLC (Kromasil RP-18, 60*2.1 mm, eluent=A: H2O+5 mL HClO4/L; B: acetonitrile; gradient=0-4.5 min 98% A-90% B; 4.5-6.5 min 90% B; 0.75 mL/min; temp.: 30 C., UV detection at 21 nm): Rt=3.51 min 1H-NMR (300 MHz in D6-DMSO) delta=5.98 (s, 2H), 6.74 (d, 1H), 7.63 (m, 1H), 8.10 (s, 1H), 12.33 (s, broad, 1H) MS (ESI+): m/z=281 [M+NH4]+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 19718-49-1, its application will become more common.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; Hendrix, Martin; Boebeta, Frank-Gerhard; Erb, Christina; Krueger, Joachim; Luithle, Joachim; Methfessel, Christoph; Schreiber, Rudy; Wiese, Welf-Burkhard; US9139579; (2015); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

19718-49-1, name is Methyl 4-amino-3-iodobenzoate, 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. name: Methyl 4-amino-3-iodobenzoate

To a stirred solution of Intermediate 14 (31.9 g, 107 mmol) in DMF (160 ml) was added methyl 4-amino-3-iodobenzoate (29.8 g 107 mmol), LiCl (4.5 g 107 mmol) and Na2CO3 (22.8 g 215 mmol). The resulting suspension was degassed, Pd(OAc)2 (0.96 g, 4.3 mmol) added, and degassing repeated. The reaction mixture was heated to HO0C for 50 minutes. The reaction mixture was then cooled to room temperature, filtered through celite and concentrated in vacuo. The resulting brown oil was separated between isopropyl acetate and water. The aqueous layer was back-extracted with isopropyl acetate (2 x 150 mL). The combined organic layers were dried (MgSO4), treated with decolourising charcoal (5% by weight of crude material) for 30 minutes at room temperature, and purified by column chromatography (SiO2, DCM) to give the title compound (9.0 g, 19%) as a pale cream solid. deltaeta (CDCl3) 8.50 (IH, br s), 8.05 (IH, s), 7.88 (IH, d), 7.32 (IH, d), 4.32 (IH, m), 3.99 (IH, t), 3.91 (3H, s), 3.65 (IH, d), 3.50-3.28 (3H, m), 3.05 (IH, dd), 1.48 (9H, s), 0.40 (9H, s). LCMS (ES+) 469.1 (M+Na).

The synthetic route of 19718-49-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UCB PHARMA S.A.; WO2009/71888; (2009); A1;,
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. 29289-13-2, name is 2-Iodo-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 29289-13-2

To a two-necked round-bottomed flask fitted with a guard tube, PBr3 (2.7mmol, 0.26 mL), DMF (3 mmol, 0.23 mL) and chloroform (0.80 mL) were added, allowed to cool to 0 C and stirred for 0.5 h. After formation of colourless solid complex, 2-Iodo-4-methyl-phenylamine 2b (1 mmol) in chloroform (5 mL) was added and the reaction mixture was allowed to stir at r.t. for another 1-2 h. After completion, the reaction mixture was neutralized by adding saturated NaHCO3 solution and then extracted with DCM (3X 20 mL). Combined organic layer was washed with brine and dried over Na2SO4. The solvent was evaporated under reduced pressure and the crude product was purified through column chromatography using silica gel (60-120 mesh) and petether/EtOAc (5:1) as eluent.

According to the analysis of related databases, 29289-13-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ghosh, Munmun; Ahmed, Atiur; Singha, Raju; Ray, Jayanta K.; Tetrahedron Letters; vol. 56; 2; (2015); p. 353 – 355;,
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. 1829-28-3, name is Ethyl 2-iodobenzoate, A new synthetic method of this compound is introduced below., Safety of Ethyl 2-iodobenzoate

0.54 g (5 mmol) of 2.76 g (10 mmol) of o-phenylenediamine and ethyl iodobenzoate were weighed into a microwave reaction tube, and cuprous iodide (80 mg, 0.5 mmol), potassium phosphate (3.18 g, 15 mmol), Then, an appropriate amount of ethylene glycol and magnetron were added to the microwave reaction tube, and the microwave reaction was carried out under the protection of nitrogen at 180 C. After 1 h, the reaction was stopped, and the TLC detection was completed. Ethyl acetate (3 × 100 mL) and an appropriate amount of water and saturated NaCl solution were extracted, the organic layer was combined, an appropriate amount of anhydrous Na 2 SO 4 was added to remove water, suction filtration, and the filtered liquid was concentrated, and 1 g of silica gel was added for mixing.Separated using silica gel column chromatography,The eluent was (dichloromethane/methanol = 100/1) to give a bright yellow solid, 3, 0.68 g, yield 65%.

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; Xinxiang Medical University; Xinxiang Medical School San Quan College; Yan Fulin; Wang Yawen; Yan Jianwei; Yin Tiantian; Ma Jinshuo; (15 pag.)CN110183387; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com