Month: May 2021

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. 141738-80-9, name is 3-Chloro-4-iodobenzotrifluoride, A new synthetic method of this compound is introduced below., Product Details of 141738-80-9

Stef> 1; A stirring mixture of 3-(3-(4-bromophenyl)propyl)-4-(2-fluorophenyl)-lH-l,2,4-triazol- 5(4H)-one (0.200 g, 0.53 mmol, Example 29, step 3), copper(I) iodide (0.010 g, 0.053 mmol), potassium carbonate (0.147 g, 1.06 mmol), L-proline (0.012 g, 0.106 mmol) and DMSO (5 mL) was sub-surface purged with nitrogen gas for 10 minutes before adding 2-chloro-4-trifluoromethyliodobenzene (0.103 mL, 0.58 mmol). The reaction vessel was stirred at 90 C for 48 h, cooled to RT, and diluted with ether and brine. The organic extract was washed sequentially with IN HQ (aq.) and water. The organic layer was then concentrated in vacuo. The resulting crude material was purified on silica gel eluting with a solvent gradient of 0% to 45% EtOAc in hexanes to afford 3-(3-(4-bromophenyl)propyl)-4-(2-fluorophenyl)-l-(2-chloro-4- (trifluoromethyl)phenyl) – 1 H- 1 ,2,4 -triazol-5 (4H) -one .

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; INCEPTION 2, INC.; STOCK, Nicholas, Simon; CHEN, Austin, Chih-Yu; BRAVO, Yalda, Mostofi; JACINTHO, Jason, Duarte; WO2015/35059; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 883546-30-3, A common heterocyclic compound, 883546-30-3, name is 2-Bromo-4-(trifluoromethoxy)iodobenzene, molecular formula is C7H3BrF3IO, 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.

A suspension of the boronic acid (360 mg, 1.6 mmol), 2-bromo-1-iodo-4-(trifluoromethoxy)benzene (575 mg, 1.6 mmol), dppf(Pd)Cl2 (57 mg, 0.078 mmol), potassium carbonate (433 mg, 3.1 mmol) in degassed toluene (4 mL), degassed water (2 mL) and degassed ethanol (2 mL) was heated at 45 C. for 3 hours. The layers were separated and the organics were concentrated and purified by column chromatography to provide the desired product.426.0 (M+1).1H NMR (CDCl3) d 8.23 (s, 1H), 7.99 (s, 1H), 7.64 (s, 1H), 7.30-7.53 (m, 3H).

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; Gilead Palo Alto, Inc.; US2011/21521; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 1155371-47-3, name is 1-Iodo-5-isopropyl-2,4-dimethoxybenzene, 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. HPLC of Formula: C11H15IO2

A suspension of 1-iodo-5-isopropyl-2,4-dimethoxybenzene (344 mg, 1.12 mmol) in freshly distilled Et3N in a screwcap vial was added Pd(PPh3)2CI2 (48 mg), CuI (68 mg, 0.36 mmol), and trimethylsilyiacetylene (0.8 ml, 5.66 mmol). The mixture was stirred at reflux overnight. The vial was then cooled to room temperature and the reaction mixture diluted with diethylether, and the organic phase was washed with a saturated solution of NH4CI and then with a saturated solution of NaHCO3. The organic phase was dried (MgSO4) and evaporated. The residue was purified by column chromatography using 5% EtOAc in petrol ether as eluent. The title compound (219 mg, 70%) was isolated as a solid. NMR (DMSO-c/e): delta 7.09 (s, 1 H), 6.61 (s, 1 H), 3.85 (s, 3H), 3.83 (s, 3H), 3.11 (m, 1 H), 1.11 (d, 6H), 0.198 (s, 9H).

The synthetic route of 1-Iodo-5-isopropyl-2,4-dimethoxybenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TOPOTARGET A/S; WO2009/66060; (2009); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, molecular formula is C6H3BrClI, 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: 13101-40-1

A mixture of 1-bromo-3-chloro-5-iodobenzene (1.5 g, 4.73 mmol), 4-(2,6-diisopropylphenyl)-1H-pyrazole (1.133 g, 4.96 mmol), 63 copper chloride dihydrate (0.161 g, 0.945 mmol), and 64 cesium carbonate (3.08 g, 9.45 mmol) was vacuumed and back-filled with nitrogen several times. 65 DMF (20 ml) was added to the reaction mixture and heated at 120 C. for 18 h. Cooled down and partitioned between EA and water and extracted with EA with a bit of NH4OH(aq). The organic portion was washed with brine and concentrated. Chromatographed on silica (DCM/Hep=2/1). Obtained white solid (73%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 13101-40-1, its application will become more common.

Reference:
Patent; UNIVERSAL DISPLAY CORPORATION; CHEN, Hsiao-Fan; (99 pag.)US2019/165284; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 835595-11-4, A common heterocyclic compound, 835595-11-4, name is 3,4-Dichloro-2-iodoaniline, molecular formula is C6H4Cl2IN, 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.

[0106] (a) To a solution of 3,4-dichloro-2-iodoaniline (example 2, 2.2 g, 7.67 mmol) in dry pyridine (8 mL) was added 4-tert-butyl-3-fluorophenylsulfonyl chloride (2.11 g, 8.43 mmol) and the reaction mixture was heated at 80 0 C for overnight. LCMS indicated presence of mono and bis-sulfonamides. 10 N aq. NaOH (3 mL) and ethanol (2 mL) were added to hydrolyze the bis-sulfonamide. The reaction mixture was then heated at 80 C for 2 h. It was cooled to r.t, excess solvent was removed in vacuo to afford a dark brown solid, diluted with DCM, washed with IN aq.HCl, and purified by flash column using hexanes: ethyl acetate mixture as an eluent on silica column to get the pure 4-tert-butyl-N-(3,4-dichloro-2- iodophenyl)-3-fluorobenzsulfonamide as an off white solid (3.5 g, 91%)

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; CHEMOCENTRYX, INC.; DAIRAGHI, Daniel; DRAGOLI, Dean, R.; KALISIAK, Jarek; LANGE, Christopher, W.; LELETI, Manmohan, Reddy; LI, Yandong; LUI, Rebecca, M.; MALI, Venkat, Reddy; MALATHONG, Viengkham; POWERS, Jay, P.; TANAKA, Hiroko; TAN, Joanne; WALTERS, Matthew, J.; YANG, Ju; ZHANG, Penglie; WO2015/84842; (2015); 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. 1000577-94-5, name is 3-Bromo-4-iodobenzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 1000577-94-5

General procedure: An oven-dried Schlenk tube was charged with a magneticstir bar, binucleophile 2-mercaptobenzimidazole 2 (1.0 mmol, 1.0 equiv), CuI(0.1 mmol, 10 mol %), phen (0.2 mmol, 20 mol %), and K2CO3 (2.0 mmol, 2equiv). The tube was capped and then evacuated and backfilled with nitrogen(3 times). Under a positive pressure of nitrogen, a solution of o-dihaloarene 1(1.05 mmol, 1.05 equiv) in DMF (3 mL) was added via syringe. The tube wassealed and allowed to stir at 120 C (monitored by TLC). After being cooled toroom temperature, EtOAc (40 mL) was added and the mixture was washedwith brine (20 mL 3). The organic phase was dried over Na2SO4 andconcentrated. The residue was purified by column chromatography on silicagel using petrol/EtOAc (10:1?3:1, v:v) as eluent to give product 3.

The synthetic route of 1000577-94-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gao, Jilong; Zhu, Jiaoyan; Chen, Lubin; Shao, Yingying; Zhu, Jiaqi; Huang, Yijia; Wang, Xiaoxia; Lv, Xin; Tetrahedron Letters; vol. 55; 22; (2014); p. 3367 – 3373;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 141738-80-9, name is 3-Chloro-4-iodobenzotrifluoride, 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. COA of Formula: C7H3ClF3I

A mixture of 0.5 g (1.6 mmol) of 3-chloro-4-iodobenzotrifluoride 0.7 g (3.8 mmol), N- Boc-piperazine, 41 mg (0.04 mmol) Tris (dibenzylideneacetone) dipalladium chloroform complex, 0.44 g (4.43 mmol) SODIUM-T-BUTOXIDE and 48 mg (0.16 mmol) tri-o- tolylphosphine in 6 ml dioxane was heated overnight at 100 C. The solution was allowed to cool to room temperature, taken up in ether (30ML) and washed with brine (25ML). The organic layer was dried over NA2SO4, filtered and the solvent was removed in vacuo. The crude oil was chromatographed over on silica gel: Eluent: Heptane-AcOEt 0-10% over 15MIN to provide the title compound (0.06g, 10%) as a brown oil, MS (m/e): 365.1 (MH+, 100%).

The synthetic route of 3-Chloro-4-iodobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2005/23260; (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. 5469-33-0, name is (Iodomethyl)cyclohexane, This compound has unique chemical properties. The synthetic route is as follows., Safety of (Iodomethyl)cyclohexane

In the same manner as in Preparation Example 70-2, the objective compound (797 mg, 56%) was obtained as a colorless oil from 4-bromo-1-((tert-butyldiphenylsilyloxy)methyl)-2-chlorobenzene and cyclohexylmethyl iodide. 1H-NMR(CDCl3): 0.82-1.75(11H, m), 1.11(9H, s), 2.45(2H, d, J=7 Hz), 4.79(2H, s), 7.03-7.11(2H, m), 7.31-7.48(6H, m), 7.61(1H, d, J=8 Hz), 7.63-7.73(4H, m)

According to the analysis of related databases, 5469-33-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US6348474; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 180624-10-6, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 180624-10-6 name is Methyl 4-amino-3-iodo-5-methoxybenzoate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Methyl 3-iodo-4-amino-5-methoxybenzoate (1.0 g, 3.25 mmol) was dissolved in triethylamine (6 mL). 1,1?-Bis(diphenylphosphino)ferrocene]dichloropalladium(II) (0.11 g, 0.16 mmol) and cuprous chloride (16 mg, 0.16 mmol) were added, and the mixture was cooled to 0 C. Trimethylsilylacetylene (0.55 mL, 3.9 mmol) was added dropwise. The mixture was warmed to RT and stirred for 1.5 h. The mixture was concentrated, then re-dissolved in EA, washed with brine, dried and concentrated. The crude material was purified by chromatography on silica gel (hexane:EA) to give 9-1 (0.27 g, 30%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 4-amino-3-iodo-5-methoxybenzoate, and friends who are interested can also refer to it.

Reference:
Patent; Alios BioPharma, Inc.; Wang, Guangyi; Beigelman, Leonid; Truong, Anh; Stein, Karin Ann; (234 pag.)US2016/244460; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 459424-72-7,Some common heterocyclic compound, 459424-72-7, name is 1,2,3-Trifluoro-4-iodobenzene, molecular formula is C6H2F3I, 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 25 mL reaction tube, Mn(OAc)3.2H2O(10 mol%), DABCO (2.5 equiv.) and a stirring bar were added. Then iodobenzene(1 mmol), phenyl acetylene (1 mmol) and PEG-400 were injected by syringe. The reaction tube was closed and transferred to a 70 C oil bath for 19-24 hours. After the reaction completed, cool down the reaction mixture to room temperature. Water (2 mL) was added and the reaction mixture was extracted with ethyl acetate and then concentrated and purified by column chromatography.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,2,3-Trifluoro-4-iodobenzene, its application will become more common.

Reference:
Article; Qi, Xinxin; Jiang, Li-Bing; Wu, Xiao-Feng; Tetrahedron Letters; vol. 57; 15; (2016); p. 1706 – 1710;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com