Month: July 2021

Adding a certain compound to certain chemical reactions, such as: 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane, 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 461-17-6, Recommanded Product: 461-17-6

Preparation of Intermediate 15.01 Step 1 To a suspension of silver nitrite (9 g, 58.5 mmol) in diethyl ether (25 mL) at 0C was added a solution of 4-iodo-1, 1, 1-trifluorobutane, 15.02 (10 g, 42.0 mmol) in diethyl ether (25 mL) slowly through an addition funnel (approx. 15 min). The resulting mixture was vigorously stirred at 0C and warmed to rt. After 50 h, the solid material was filtered off through a celite pad. The resulting diethyl ether solution was concentrated in vacuo to give 15.03 as colorless oil, which was used without further purification.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; SCHERING CORPORATION; WO2005/85242; (2005); 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. 191348-14-8, name is 2-Iodo-4-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 191348-14-8

General procedure: In a flame-dried flask, AlMe3 (2 M in toluene, 1.11 mL, 2.18mmol, 1.2 equiv) was added to dry toluene (3.0 mL) under anitrogen atmosphere. The mixture was cooled to 0 C, and the2-iodoaniline (2.0 mmol, 1.1 equiv) in dry toluene (4.0 mL) was added. The mixture was stirred for a further 5 min at 0 C. Theice bath was removed, and the mixture was stirred for 20 min atroom temperature. The mixture was cooled to 0 C again, and cyclopentene carboxylate 2b (1.82 mmol, 1.0 equiv) in drytoluene (3.0 mL) was added dropwise over 2 min to the mixture. After stirring for 10 min at 0 C, the mixture was heated to 60 C, and stirring was continued for 16 h. After cooling to room temperature, HCl (1 M, 8.0 mL) was added. (Caution: gas evolution,exotherm.) The mixture was stirred for 15 min, then water (20 mL) and EtOAc (30 mL) were added. The mixture was extracted, the organic phase was separated, and the aqueous phase was re-extracted one more time with EtOAc (30 mL). Thecombined organic phases were washed with brine and dried (MgSO4). After filtration, the solvent was removed under reduced pressure, and the crude mixture was purified by 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 191348-14-8.

Reference:
Article; Adeyemi, Ahmed; Wetzel, Alexander; Bergman, Joakim; Branalt, Jonas; Larhed, Mats; Synlett; vol. 30; 1; (2019); p. 82 – 88;,
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. 25309-64-2, name is 1-Ethyl-4-iodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Ethyl-4-iodobenzene

General procedure: An appropriate phenylacetamide (0.12 mmol, 1 equiv), an appropriate iodo compound (0.48 mmol, 4 equiv), Pd(OAc)2 (2.7 mg, 10 mol%), and AgOAc (50 mg, 0.3 mmol, 2.5 equiv) in anhydrous toluene (3 mL) was heated at 110 C for 24 h under a nitrogen atmosphere. After the reaction period, the solvent was evaporated in vacuo to afford a crude reaction mixture. Purification of the crude reaction mixture by column chromatography furnished the corresponding arylated products 4a-q/7a-f (bis arylation products), 3o,r/6a,b/8e,f/9a,b (mono arylation products) (see corresponding Tables/Schemes for specific examples and reaction conditions).

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; Bisht, Narendra; Babu, Srinivasarao Arulananda; Tetrahedron; vol. 72; 39; (2016); p. 5886 – 5897;,
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. 6293-83-0, name is 2-Iodo-4-nitroaniline, A new synthetic method of this compound is introduced below., COA of Formula: C6H5IN2O2

7V-Benzyl-5-bromo-2-iodobenzamide (805 mg, 1.93 mmol), 2-iodo-4-nitroaniline (425 mg, 1.61 mmol), copper(I) iodide (123 mg, 0.65 mmol), and potassium carbonate (1.11 g, 8.0 mmol) were taken up in anhydrous DMSO (1 1 mL). The resulting reaction mixture was first stirred at 80C for 2 hr, followed by heating to 135 C for another 16 hr. After cooling to room temperature, the mixture was diluted with an excess of EtzO and washed with water. The organic layer was dried over NazSOr, filtered and concentrated. The residue was purified by flash column chromatography (EtOAc : Hex = 0 : 100 to 100 : 0) to give 10-benzyl -2-bromo-8- nitro-5,10-dihydro- 1 1/7-dibenzo[£>,e][l ,4]diazepin-l l-one (179 mg, 26 %). -5if -dibenzo[6,e][l,4]

The synthetic route of 6293-83-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DANA-FARBER CANCER INSTITUTE, INC.; GRAY, Nathanael S.; DE CLERCQ, Dries; JANG, Jaebong; JANNE, Pasi; TO, Ciric; ECK, Michael; PARK, Eunyoung; HEPPNER, David; (0 pag.)WO2019/164949; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, 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: 328-73-4

General procedure: A mixture of trisallene 3 (0.25 mmol), aryl/hetereoaryl iodides (0.90 mmol), nucleophiles (0.90 mmol), Pd2(dba)3 (2.5 mol percent), TFP (tri-(2-furyl)phosphine) (10 mol percent), and K2CO3 (1.5 mmol) in MeCN (5 mL) was stirred and heated at 80 °C (oil bath temperature) until the starting material was completely consumed as monitored by TLC (see Table 1). The mixture was worked up as mentioned in general procedure A.

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

Reference:
Article; Gu?ltekin, Zeynep; Elboray, Elghareeb E.; Aly, Moustafa F.; Abbas-Temirek, Hussien H.; Shepherd, Helena J.; Grigg, Ronald; Tetrahedron; vol. 70; 33; (2014); p. 4934 – 4941;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 460-37-7, 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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows.

To zinc dust (3.24 g, 49.5 mmol, 3.41 eq) in a nitrogen-purged 40 mL vial with stir bar were added trimethylsilyl chloride (100 muL, 120 mg, 1.1 mmol, 8 mol %) and 1,2-dibromoethane (100 muL, 220 mg, 1.2 mmol, 8 mol %) by syringe. Anhydrous THF (16 mL) was added, followed by 1-iodo-3,3,3-trifluoropropane (3.8 g, 17.0 mmol, 1.17 eq) portionwise at RT with stirring over 20 min, keeping the exotherm below 50 C. The suspension was then stirred for 1 h at 50 C. To a separate 100 mL round bottom flask purged with nitrogen containing a stir bar were added RuPhos (655 mg, 1.40 mmol, 10 mol %), Pd2dba3 (629 mg, 0.687 mmol, 5 mol %), and DMF (20 mL). This was stirred for 30 min at 23 C. Trans-2-bromo-1-methylvinyl MIDA boronate (Aldrich cat. no. 763853, 3.79 g, 14.5 mmol, 1.00 eq) was then added to this solution in 13 mL DMF. The alkyl zinc suspension was filtered through a syringe filter and the filtrate was added to the DMF solution. The remaining alkylzinc solution was washed over with additional THF (2 mL). The reaction was then stirred for 24 h at 50 C., after which time nearly complete conversion of the vinyl bromide was observed by TLC (Cis plate, 2:1 H2O:MeCN, KMnO4 stain). In a separatory funnel, the reaction was diluted with EtOAc and saturated aqueous NH4Cl was added. The aqueous phase was extracted twice with EtOAc. The combined organic phase was washed three times with H2O, each time adding a few mL of brine to break the emulsion. The organic phase was dried with Na2SO4, concentrated to a dark orange foam, then dissolved in DCM and adsorbed onto celite. The celite pad was loaded onto a Cis silica column of 100 mL volume, eluting with a gradient of 30% to 60% MeCN in H2O. The product-containing fractions were combined and solid NaCl was added to induce phase separation. The organic phase was separated and the aqueous layer extracted with EtOAc (×2). The combined organic phases were dried and concentrated to give SI-10 as a yellow solid (2.91 g, 9.93 mmol 68% yield). (0225) 1H NMR (500 MHz, CDCl3) delta 5.87 (t, J=7.2 Hz, 1H), 3.81 (d, J=16.3 Hz, 2H), 3.69 (d, J=16.3 Hz, 2H), 2.79 (s, 3H), 2.41 (q, J=7.3 Hz, 2H), 2.27-2.14 (m, 2H), 1.68 (dt, J=1.6, 0.9 Hz, 3H). 13C NMR (126 MHz, CDCl3) delta166.90, 136.96, 61.77, 46.25, 33.06 (q, JC-F=27.7 Hz), 21.23 (q, JC-F=2.5 Hz), 14.39. 19F NMR (470 MHz, CDCl3) -66.33 (t, J=11.0 Hz). 11B NMR (128 MHz, CDCl3) delta 11.02. HRMS (ES+) Calculated for C11H16NO4BF3: 294.1124; Found: 294.1121.

The chemical industry reduces the impact on the environment during synthesis 1,1,1-Trifluoro-3-iodopropane. I believe this compound will play a more active role in future production and life.

Reference:
Patent; The Board of Trustees of the University of Illinois; BURKE, Martin D.; CROUCH, Ian; LEHMANN, Jonathan; PALAZZOLO, Andrea; SIMONS, Claire; US2018/305381; (2018); 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. 13194-68-8, name is 4-Iodo-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 4-Iodo-2-methylaniline

EXAMPLE 3; Synthesis of (3); A flask is charged with 100 mmol of boric acid followed by 6N HCl solution to adjust the reaction solution to a pH of 2. Once the salt dissolves, 20 mmol of 4-iodo-2-methylaniline is added to the reaction solution, followed by enough ice to reduce solution temperature to 0 C. In a separate flask, 20 mmol of sodium nitrite (NaNO2) is dissolved in ice water. The NaNO2 solution is added drop-wise with constant stirring to the 4-iodo-2-methylaniline solution. The pH of the reaction solution is maintained by addition of 6N HCl. After the NaNO2 solution addition is complete, ice is added to maintain the 0 C. reaction temperature. A 3rd flask is charged with 20 mmol of p-cresol, water and 2.5 N NaOH (20 mmol), which is then added drop wise to the ice cooled reaction with constant stirring. The reaction mixture is allowed to stir for 15 min at pH 2.0-2.5. NaOH (2.5 N) is then added in small aliquots to the reaction solution to increase the pH to 8.5. The reaction solution is allowed to warm to room temperature. Dibasic sodium phosphate solution (100 mmol) is added and the pH is adjusted to 6.0 with 6 N HCl. The product is filtered, rinsed with ice water and air dried. The product is purified by column chromatography to yield 2-(4-iodo-2-methyl-phenylazo)-4-methyl-phenol (3).

According to the analysis of related databases, 13194-68-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALCON, INC.; US2009/43105; (2009); 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. 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, A new synthetic method of this compound is introduced below., Product Details of 5876-51-7

General procedure: 4.2. Experimental procedure for the synthesis of 3: A solution of the indole 1 (1 mmol), aryl halide 2 (1.5 mmol), CuI (0.1 mmol, 10 mol %), metformin hydrochloride (0.2 mmol, 20 mol %), Cs2CO3 (2 mmol, 2 equiv), and DMF (2 mL) was heated to 130 C under N2. The reaction mixture was stirred for the appropriate time (Table 4), and the progress of the reaction was followed by TLC. After completion of the reaction, the mixture was cooled to room temperature, and diluted with EtOAc (10 mL). The solid was removed by filter, and the filtrate was washed with water and brine.The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography to afford the product 3.

The synthetic route of 5876-51-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Hu; Lei, Min; Hu, Lihong; Tetrahedron; vol. 70; 35; (2014); p. 5626 – 5631;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 6213-88-3, A common heterocyclic compound, 6213-88-3, name is (E)-Methyl 3-iodoacrylate, molecular formula is C4H5IO2, 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.

Methyl (2E)-3-iodoprop-2-enoate (0.141 g, 0.665 mmol), Pd(OAc)2 (15 mg, 0.067 mmol), ligand (0.13 mmol) and AgOAc (0.120 g, 0.721 mmol) were added to dry flasks under argon in the absence of light. Degassed MeCN (4.0 mL) was added to each flask, followed by 4,4,6-trimethyl-2-vinyl-1,3,2-dioxaborinane (0.13 mL, 0.76 mmol) under a positive pressure of argon. The flasks were then purged with argon for 2 min, and then stirred vigorously at room temperature, with conversion monitored at 1.5 h, 3 h and 24 h by 1HNMR. The HM:SM ratio was also determined by 1H NMR spectroscopy.

The synthetic route of 6213-88-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Madden, Katrina S.; Knowles, Jonathan P.; Whiting, Andrew; Tetrahedron; vol. 75; 45; (2019);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 32024-15-0, These common heterocyclic compound, 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde, 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: K2CO3 (2.5 × 10-4 mol, 2.5 equiv), aryl iodide (1.0 × 10-4 mol, 1.0 equiv), and alkyne (1.5 × 10-4 mol, 1.5 equiv) were mixed in a 10-mL vial, followed by addition of a solution of the selected catalyst (1 × 10-8 mol) in EtOH (1 mL). The vial was placed in a preheated oil bath at 80 C and stirred for 1 h. After cooling to 20-25 C, the reaction mixture was evaporated to dryness under a stream of dinitrogen followed by addition of 1.0 equiv of 1,2-dimethoxyethane as NMR internal standard, and extraction of the reaction mixture with three 0.20-mL portions of CDCl3. All fractions were joined and analyzed by 1H NMR spectroscopy. The product peak assignments were based on the authentic samples or on published dat, whereas quantifications were performed upon integration of the selected peak of the product relatively to the peak of the standard.

Statistics shows that 3-Iodo-4,5-dimethoxybenzaldehyde is playing an increasingly important role. we look forward to future research findings about 32024-15-0.

Reference:
Article; Timofeeva, Svetlana A.; Kinzhalov, Mikhail A.; Valishina, Elena A.; Luzyanin, Konstantin V.; Boyarskiy, Vadim P.; Buslaeva, Tatyana M.; Haukka, Matti; Kukushkin, Vadim Yu.; Journal of Catalysis; vol. 329; (2015); p. 449 – 456;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com