Month: May 2021

Synthetic Route of 42048-11-3, 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. 42048-11-3, name is 2-Chloro-6-iodotoluene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Palladium acetate palladium (44.9 mg, 0.2 mmol) was added to a 25 mL eggplant bottle.Triphenylphosphine (52.4 mg, 0.2 mmol),Sodium formate (276 mg, 4 mmol),Norbornene (188 mg, 2 mmol),Potassium phosphate (2.544 g, 12 mmol),Potassium acetate (392 mg, 4 mmol),2-chloro-6-sulfonic acid toluene (504 mg, 2 mmol),Ethyl bromobutyrate (1.56 g, 8 mmol) and dimethylformamide (10 ml).High-purity nitrogen was replaced three times, after reacting at 50oC for 16 hours,Extracting the mixture with dichloromethane and water, combining the organic phases, enriching the organic solvent, and further purifying the product by column chromatography. 2-Deutero-3-(ethyl butyrate)-6-chlorotoluene was obtained in a yield of 78%.

The synthetic route of 2-Chloro-6-iodotoluene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anhui Xiulang New Materials Technology Co., Ltd.; Zhang Honghai; Guo Lei; Shui Xinfeng; (15 pag.)CN110054541; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 1000802-34-5, A common heterocyclic compound, 1000802-34-5, name is 6-Iodobenzo[d][1,3]dioxol-5-amine, molecular formula is C7H6INO2, 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.

To a solution of 6-iodobenzo[d][1,3]dioxol-5-amine (1 g, 3.8 mmol) and paraformaldehyde (1.14 g, 38 mmol) in methanol (10 mL) was added NaBH3CN (2.39 g, 38 mmol) slowly with stirring. The mixture was heated to 50 C. for 4 h. Water (100 mL) was added and extracted with methylene chloride (100 mL). The organic layer was washed with brine (100 mL), dried (MgSO4) and evaporated under vacuum to give crude title compound 0107-111 (1.16 g) as a brown oil which was used directly to the next step without further purification. LCMS: 292 [M+1]+; 1H NMR (DMSO-d6) delta 2.56 (s, 6H), 6.02 (s, 2H), 6.96 (s, 1H), 7.32 (s, 1H).

The synthetic route of 1000802-34-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Cai, Xiong; Qian, Changgeng; Zhai, Haixiao; US2008/234314; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 1097871-23-2,Some common heterocyclic compound, 1097871-23-2, name is 1-Chloro-2,5-difluoro-4-iodobenzene, molecular formula is C6H2ClF2I, 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 2: Preparation of (S)-N-(-(4-chloro-2,5-difluorophenyl)(oxetan-3-yl)methyl)-2-methylpropane-2-sulfinamide To an oven-dried 500 mL round bottom flask under a nitrogen atmosphere was added 1-chloro-2,5-difluoro-4-iodobenzene (9.93 g, 36.18 mmol) in 175 mL anhydrous THF. The resulting solution was cooled to -100 C. with a diethyl ether/liquid nitrogen bath, and then n-BuLi solution (1.6M in THF, 22.6 mL, 36.2 mmol) was added dropwise so that the internal temperature remained between -90 and -100 C. The resulting yellow colored mixture was stirred between -90 and -100 C for 30 min and then (S,E)-2-methyl-N-(oxetan-3-ylmethylene)propane-2-sulfinamide (7.53 g, 39.80 mmol) in 15 mL THF was added dropwise via syringe so that the internal temperature remained between -90 and -100 C. The resulting mixture was stirred between -90 and -100 C. for 30 min and then quenched at the same temperature by dropwise addition of saturated NH4Cl solution followed by warming to room temperature. The mixture was diluted with 150 mL water and 150 mL EtOAc. The layers were shaken and separated and the organic phase was washed with saturated NaCl solution, dried over Na2SO4, and concentrated to a viscous nearly colorless oil which was purified by MPLC using silica gel (0-100% ethyl acetate/hexanes) to provide the desired single diastereomer (6.88 g, 20.38 mmol) as a white foam. LCMS-APCI (POS.) m/z: 338.1 (M+H)+

The synthetic route of 1097871-23-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMGEN INC.; CYTOKINETICS, INC.; Ashcraft, Luke; Boezio, Alessandro; Butler, John; Chandra, Aroop; Chuang, Chihyuan; Collibee, Scott E.; Debenedetto, Mikkel; DiMassa, Vincent; Graceffa, Russell; Malinowski, Justin; Moebius, David; Morgan, Bradley P.; Payette, Joshua; Romero, Antonio; St. Jean, JR., David; Vargas, Richard; Yeoman, John; Zhang, Hanmo; (146 pag.)US2019/77793; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 404337-42-4, A common heterocyclic compound, 404337-42-4, name is 5-Chloro-2-iodo-m-xylene, molecular formula is C8H8ClI, 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.

4-Chloro-2,6-dimethyliodobenzene (9.6 g, 36 mmol) is dissolved in pyrene (60 mL). To this solution, a hot solution of KMnO4 (28 g, 0.18 mol) is poured and the mixture is stirred at 115 C. for 8 hours. After additional heating for 5 hours, a 1M HCl solution is added. The precipitate is filtered off and washed with THF. The resultant filtrate is washed with THF and dried over Na2SO4. After the evaporation, the dicarboxylic acid derivative is obtained as a solid. Yield 9.1 g (78%). FD-MS (8 kV): m/z=326.7. 1H NMR (250 MHz, DMSO-d6) delta ppm 7.24 (s, Ar): 13C NMR (62.5 MHz, CD3OD-d4): delta ppm 126.7, 128.1, 134.5, 150.1, 174.6.

The synthetic route of 404337-42-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; Kawano, Shin-Ichiro; Baumgarten, Martin; Muellen, Klaus; Murer, Peter; Schaefer, Thomas; Saleh, Moussa; US2014/357898; (2014); A1;,
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 914636-93-4 as follows. Computed Properties of C7H4FIO

Step 5. (R,E)-N-(3-fluoro-5-iodobenzylidene)-2-methylpropane-2-sulfinamide To a solution of 3-fluoro-5-iodobenzaldehyde (8.75 g, 35 mmol) and (R)-(+)-t-Butylsulfinamide (4.67 g, 38.5 mmol) in DCE (117 mL) was added copper(II) sulfate (anhydrous) (16.76 g, 105 mmol) and the resulting suspension was heated at 60° C. overnight. LCMS indicated desired product formation. Reaction mixture was filtered through Celite and the filtrate concentrate in vacuo and then taken to the next step as such. LCMS (m/z): 354.1 (MH+), 1.08 min.

According to the analysis of related databases, 914636-93-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Novartis AG; Bagdanoff, Jeffrey T.; Ding, Yu; Han, Wooseok; Huang, Zilin; Jiang, Qun; Jin, Jeff Xianming; Kou, Xiang; Lee, Patrick; Lindvall, Mika; Min, Zhongcheng; Pan, Yue; Pecchi, Sabina; Pfister, Keith Bruce; Poon, Daniel; Rauniyar, Vivek; Wang, Xiaojing Michael; Zhang, Qiong; Zhou, Jianguang; Zhu, Shejin; (366 pag.)US9242996; (2016); 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. 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-3-chloro-5-iodobenzene

In a 250mL three-necked flask, nitrogen is introduced.Add 0.02molRaw material I, 150ml DMF, 0.022mol raw material II,0.0002 mol of palladium acetate, stirred,Then add 3mL of 0.01mol/mL K3PO4 aqueous solution,The reaction was heated under reflux at 150 C for 12 hours.Sampling the plate and the reaction is complete.Cool naturally, add 100mL water,The mixture was filtered and the filter cake was dried in a vacuum oven.The residue obtained was purified by silica gel column to giveRaw material A-1;

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; Jiangsu March Optoelectric Technology Co., Ltd.; Lu Ying; Wang Fang; Xie Dandan; Wu Xiuqin; Zhang Zhaochao; (39 pag.)CN109928911; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 1032231-24-5, A common heterocyclic compound, 1032231-24-5, name is 2-Bromo-5-iodobenzaldehyde, molecular formula is C7H4BrIO, 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.

According to the method described in a journal, European Journal of Organic Chemistry, 2008, No. 10, pp. 1797-1801, a compound represented by the formula (I-9-3) was produced. In a nitrogen atmosphere, 2.0 g of the compound represented by the formula (I-9-2), 3.0 g of the compound represented by the formula (I-9-3), 2.0 g of potassium carbonate, 20 mL of tetrahydrofuran, 20 mL of water, and 0.1 g of tetrakis(triphenylphosphine)palladium(0) were put in a reactor and heated with stirring. After ordinary post-treatment, this was purified through column chromatography to give 2.3 g of a compound represented by the formula (I-9-4).

The synthetic route of 1032231-24-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DIC Corporation; Horiguchi, Masahiro; Kadomoto, Yutaka; (139 pag.)US2018/22716; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 90064-47-4,Some common heterocyclic compound, 90064-47-4, name is 4-Iodo-2,5-dimethoxybenzaldehyde, molecular formula is C9H9IO3, 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 DMAc solution (30 mL) of 6 (1.0 g, 1.66 mmol),4-iodo-2,5-dimethoxybenzaldehyde (0.63 g, 2.16 mmol),sodium carbonate (0.53 g, 4.99 mmol), 2,6-di-tertbutyl-p-cresol (0.07 g, 0.33 mmol), and trans-di(-acetato)bis[o-(di-o-tolylphosphino)benzyl] dipalladium(II)(16 mg, 0.017 mmol) was stirred at 110 C for 16 h.After removal of the solvent, the mixture was poured intomethylene chloride and washed with water. After removalof the organic solvent, the residue was purified by columnchromatography on a silica gel using methylene chlorideand n-hexane (1:5, v/v) as an eluent. Yield (550 mg,43%). mp 254-257 C. 1H NMR (400 MHz, DMSO-d6) 3.90 (s, 3 H, -Ph-O-CH3), 3.98 (s, 3 H, -Ph-O-CH3),7.20 (s, 1 H, CHO-Ph-CH ), 7.29 (t, J = 7.7 Hz, 4H,-Ph-carbazole), 7.30 (d, J = 16.5 Hz, 1 H, -CH CH-),7.35 (s, 1 H, CHO-Ph-CH ), 7.40 (d, J = 8.8 Hz, 2 H,CH-Ph-N-), 7.43 (t, J = 7.7 Hz, 4 H, -Ph-carbazole),7.45 (d, J = 16.5 Hz, 1 H, -CH CH-), 7.47 (d, J =8.8 Hz, 4 H, -N-Ph-carbazole), 7.50 (d, J = 8.8 Hz,4 H, -N-Ph-carbazole), 7.53 (d, J = 7.7 Hz, 4 H, -Ph-carbazole), 7.59 (d, J = 8.8 Hz, 2 H, CH-Ph-N-), 8.16(d, J = 7.7 Hz, 4 H, -Ph-carbazole), 10.4 (s, 1 H, -Ph-CHO); 13C NMR (100.64 MHz, DMSO-d6) 56.12,56.24, 109.15, 109.72, 111.09, 115.14, 119.84, 120.18,123.25, 124.29, 125.20, 125.83, 128.05, 128.18, 132.35,132.61, 136.58, 140.85, 142.37, 146.15, 147.21, 187.91,161.18, 156.94, 187.94.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Iodo-2,5-dimethoxybenzaldehyde, its application will become more common.

Reference:
Article; Lee, Jeonghun; Im, Hunbae; Kim, Sukwon; Kim, Chulhee; Journal of Nanoscience and Nanotechnology; vol. 15; 2; (2015); p. 1434 – 1442;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 264927-52-8, These common heterocyclic compound, 264927-52-8, name is 2-Chloro-4-fluoro-5-iodobenzoic 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.

b Methyl 2-chloro-4-fluoro-5-iodobenzoate 30.8 g of 2-chloro-4-fluoro-5-iodobenzoic acid were dissolved in 300 ml of MeOH and 36 ml of thionyl chloride were added dropwise. The mixture was refluxed for 4 hours and the volatile constituents were removed in vacuo. The residue was taken up using 600 ml of EA and washed with 400 ml of a half-concentrated aqueous Na2 CO3 solution. The organic phase was dried over Na2 SO4 and the solvent was removed in vacuo. The residue was stirred with 200 ml of HEP, and the precipitate was filtered off and washed with 100 ml of HEP. 5.8 g of methyl 2-chloro-4-fluoro-3,5-diiodobenzoate were obtained, mp 155 C. The solvent was removed in vacuo from the filtrate containing the desired product and 23.5 g of white crystals were obtained, mp 52 C.

The synthetic route of 264927-52-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoechst Aktiengesellschaft; US6057322; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 180624-10-6, 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. 180624-10-6, name is Methyl 4-amino-3-iodo-5-methoxybenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[1423] To a stirring mixture of 642-1 (540 mg, 1 .76 mmol) in DMF (5 mL, deoxygenated prior to use) were added Pd(OAc)? (1 19 mg, 0.1 7 mmol), PPh3 (102 mg. 0.387 mmol), TEA (0.3 mL, 2.1 1 mmol) and ethyl acrylate (0.42 mL, 3.87 mmol). The mixture was stirred at 85 C overnight. The mixture was diluted with EtOAc and washed with brine. The layers were separated, and the aqueous layer was extracted with EtOAc. The organic layers were dried over Na2SC>4, filtered and concentrated under reduced pressure. The crude product was purified via a silica gel chromatography to afford 642-2 as a yellow solid (410 mg, 83%). LCMS: m/z 280.05 [M+H]+.

The synthetic route of Methyl 4-amino-3-iodo-5-methoxybenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALIOS BIOPHARMA, INC.; WANG, Guangyi; BEIGELMAN, Leonid; TRUONG, Anh; NAPOLITANO, Carmela; ANDREOTTI, Daniele; HE, Haiying; STEIN, Karin, Ann; WO2015/26792; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com