Author: Jessica.F

60577-34-6, name is 4-Iodo-N-methylaniline, 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. SDS of cas: 60577-34-6

To a 250?mL round-bottomed flask equipped with a magnetic stir bar was added 4-iodo-N-methylaniline (2, 35.0?g, 150? mmol, 1 equiv) and 100?mL DCM. tBuONO (26.8?mL, 225?mmol, 1.5 equiv) was added dropwise into the flask under ice bath in 15?min. Then the reaction was allowed to proceed under stirring at r.t. for 4?h until the completion of reaction. The solvent was removed under reduced pressure and the residue was purified by flash column chromatography on silica gel with PE/EA (4:1) as the eluent and recrystallized in PE and DCM. The product 3 was obtained as a light yellow solid in 94% yield (37.0?g, 141?mmol). 1H NMR (500?MHz, CDCl3) delta 7.82-7.77 (m, 2H), 7.34-7.29 (m, 2H), 3.42 (s, 3H). 13C NMR (126?MHz, CDCl3) delta 142.01, 138.50, 120.53, 91.62, 30.97.

The synthetic route of 60577-34-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Zhongsu; Zeng, Hua; Zhang, Wenjing; Song, Chao; Yang, Fan; Liu, Yun; Zhu, Jin; Polymer; vol. 172; (2019); p. 152 – 159;,
Iodide – Wikipedia,
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These common heterocyclic compound, 1094759-93-9, name is 4-Chloro-5-fluoro-2-iodoaniline, 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. Application In Synthesis of 4-Chloro-5-fluoro-2-iodoaniline

To Intermediate 5A (47g, 17.3 mmol) in AcOH (470 mL) was added NaN3 (33.76g, 51.9 mmol) and trimethyl orthoformate (56.8 mL, 51.9 mmol). After 30 h, the reaction was poured into ice H2O, the solids were filtered-off and washed with petroleum ether to afford 49 g Intermediate 5B. MS (ESI) m/z: 324.8 (M+H)+.

The synthetic route of 4-Chloro-5-fluoro-2-iodoaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ORWAT, Michael J.; PINTO, Donald J.P.; SMITH II, Leon M.; SRIVASTAVA, Shefali; WO2013/56060; (2013); 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. 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, A new synthetic method of this compound is introduced below., name: 2-(2-Iodophenyl)acetonitrile

General procedure: A flask was equipped with a magnetic stir bar and charged with 1Hpyrrole-2-carbaldehyde (2a; 19.0 mg, 0.2 mmol, 1.0 equiv), 2-bromophenylacetonitrile(1a; 39.2 mg, 0.2 mmol, 1.0 equiv), and K3PO4(63.6 mg, 0.3 mmol, 1.5 equiv). The flask was evacuated and filledwith N2, and then anhydrous DMSO (2.0 mL) was introduced via a syringe.The flask was heated in a 130 C oil bath for 24 h, at which timeTLC analysis [petroleum ether (bp 60-90 C)-EtOAc, 10:1] indicatedcomplete consumption of 2a and 1a. The reaction mixture was cooledto r.t. and added to a sat. solution of NaCl (20 mL) and extracted withEtOAc (3 ¡Á 10 mL). The combined organic layers were dried (Na2SO4)and filtered. The filtrate was concentrated, and the residue was purified by column chromatography on SiO2 [petroleum ether (bp 60-90C)-EtOAc, 10:1 to 30:1] to give 3ad; Yield: 40.5 mg (84%); fluorescent yellow solid; mp 193.7-194.6 C.

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; Jiang, Zeng-Qiang; Miao, Da-Zhuang; Tong, Yao; Pan, Qiang; Li, Xiao-Tong; Hu, Ren-He; Han, Shi-Qing; Synthesis; vol. 47; 13; (2015); p. 1913 – 1921;,
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. 618-91-7, name is Methyl 3-iodobenzoate, A new synthetic method of this compound is introduced below., Application In Synthesis of Methyl 3-iodobenzoate

General procedure: A mixture ofmethyl 3-iodobenzoate (1 mmol), corresponding amine (3 mmol), K2CO3(4 mmol), CuI (0.2 mmol) and L-proline (0.4 mmol) in 15 mL of DMSO was heatedat 60 C for 8 h. The cooled mixture was pour into 150 ml water, and extractedwith ethyl acetate (3 ¡Á 15 mL), the organic fractions were combined, washedwith saturated brine (2 ¡Á 15 ml) prior to drying over anhydrous sodium sulfate.After filtration and concentrate using a rotary evaporator, the residue was purified by silica gel column chromatographyusing a mixture of petroleum ether/ethyl acetate (20 : 1, v/v) as eluent toafford the desired product.

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; Li, Zheng; Pan, Miaobo; Su, Xin; Dai, Yuxuan; Fu, Mian; Cai, Xingguang; Shi, Wei; Huang, Wenlong; Qian, Hai; Bioorganic and Medicinal Chemistry; vol. 24; 9; (2016); p. 1981 – 1987;,
Iodide – Wikipedia,
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112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, 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: 4-Bromo-1-iodo-2-nitrobenzene

Dissolving 50 g of 2-naphthalene boronic acid, 94 g of 2-nitro-4-bromo-1-iodobenzene, and 10 g of Pd(PPh3)4 In a mixed solvent of 300 mL of THF and 50 mL of H2O, the mixture was reacted at 80 C for 24 hours under a nitrogen atmosphere. The solvent was dried and extracted with dichloromethane.Washing liquid, column chromatography to obtain intermediate M2.

The synthetic route of 112671-42-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou Huarui Optoelectric Materials Co., Ltd.; Pan Junyou; Zhang Chen; Jiang Guangtao; You Xueqiang; Huang Hong; (40 pag.)CN109705100; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 61203-48-3, 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. 61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of benzonitrile(2.0 mmol) and o-iodobenzoic acid (2.0 mmol) and [bmIm]OH (35mol) was stirred at room temperature for (3-5) h. After completion of reaction as indicated byTLC, 20mL of water was added to the reaction mixture and stirred well. The product was extracted with ether (3¡Á20 mL). The combined organic layers were dried over anhydrous Na2SO4 to afford the crude product, this crude product was taken to column in order to obtain analytically pure compound 4(a-m)(77-91%). After isolation of the product, the remaining aqueous layer containing the ionic liquid was washed with ether (2x10mL) to remove organic impurity and filtered. The filtrate was extracted with dichloromethane(2¡Á10mL), dried over MgSO4 and evaporated under reduced pressure to afford [bmIm]OH, which was reused five times in subsequent runs without further purification.

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

Reference:
Article; Waseem, Malik Abdul; Shireen; Srivastava, Anjali; Srivastava, Arjita; Rahila; Siddiqui; Tetrahedron Letters; vol. 55; 44; (2014); p. 6072 – 6076;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 619-58-9, 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. 619-58-9, name is 4-Iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Method B.A solution of 4-methoxyphenyl boronic acid (1 g, 6.58 mmol), 4-iodobenzoic acid (1.63 g, 6.58 mmol) and cesium carbonate (5.36 g, 16.45 mmol) in 3:1 1,2- dimethoxyethane/water was deoxygenated with nitrogen for 15 minutes. Pd(PPtLs)4 (380 mg, 0.329 mmol) was then added and the solution was heated to 80 C for 6h. The reaction was allowed to cool and acidified with 2M HCl which caused a precipitate to form. The precipitate was filtered and the filtrate was extracted twice with dichloromethane. The organic layer was then dried over magnesium sulfate, filtered through diatomaceous earth filter aid (CELITE) and evaporated under reduced pressure to yield a combined 1.5O g (95%). 1HNMR (DMSO): delta 7.99 (d, J=8.4 Hz, 2H), 7.74 (d, J=8.4 Hz, 2H), 7.69 (d, J=8.7 Hz, 2H), 7.04 (d, J=8.7 Hz, 2H), 3.80 (s, 3H). 13CNMR (DMSO): delta 167.17, 159.49, 143.90, 131.16, 129.91, 128.77, 128.09, 126.08, 114.45, 55.17.

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

Reference:
Patent; GEORGETOWN UNIVERSITY; WO2009/146013; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 156150-67-3,Some common heterocyclic compound, 156150-67-3, name is 2-Chloro-1-fluoro-4-iodobenzene, molecular formula is C6H3ClFI, 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.

Example 22 : 5-([l ,2,4] triazolo [1 ,5-a] pyridin-6-yl)-4-(3-chloro-4-fluorophenyl)-2,2- dimethylfuran-3(2H)-one; [00195] Cesium acetate (167 mg, 0.000872 mol) was added to a round bottom flask and dried under vacuum at 125 C for 2 hours. Palladium acetate (0.98 mg, 0.0000044 mol), tris(4-trifluoromethylphenyl)phosphine (8.1 mg, 0.000017 mol), and N,N- dimethylformamide (1.7 mL, 0.022 mol) were added to the dried cesium acetate and the mixture stirred for 30 min. 5-([l,2,4]triazolo[l,5-a]pyridin-6-yl)-2,2-dimethylfuran-3(2H)- one (100.0 mg, 0.0004362 mol) and 2-chloro-l-fluoro-4-iodobenzene (112 mg, 0.000436 mol) in N,N-dimethylformamide (1.7 mL, 0.022 mol) were added and the mixture stirred at 125 0C for 18 hr. The mixture was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over sodium sulfate, filtered, and concentrated to give a yellow oil. The yellow oil was purified on HPLC eluting with acetonitrile: water (0.1% TFA) to give 20.0 mg (12.8%) of the title compound as a yellow solid.1H NMR (300 MHz, Methanol-^) delta 9.19 (s, IH), 8.49 (s, IH), 7.75 (m, 3H), 7.29 (m, 2H), 1.59 (s, 6H). MS (ESP+) m/z 358.09.

The synthetic route of 156150-67-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOGEN IDEC MA INC.; WO2008/94574; (2008); A2;,
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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C6H3BrINO2

To a solution of 4-bromo-1 -iodo-2-nitrobenzene (66 g, 0.2 mol) in MeOH (700 mL) was added stannous chloride (226 g, 1 mol) at 0 C. The resultant mixture was heated to reflux (80 C) for 4 h. The solvent was removed under reduced pressure, and then the residue was diluted with ethyl acetate (1 L), washed with H2O (1 L), dried over sodium sulfate, concentrated to give a residue which was purified by column chromatography (eluent: petroleum ether: ethyl acetate= 20:1 ) to give 5-bromo-2-iodoaniline (39 g, 65%) as a white solid. LCMS (Method B): 2.27 min m/z [MH]+=298.1 ; 300.1

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; CATALYST THERAPEUTICS PTY LTD; BURNS, Chris; GARNIER, Jean-Marc; SHARP, Phillip Patrick; FEUTRILL, John; CUZZUPE, Anthony; (140 pag.)WO2017/20086; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

34883-46-0, name is 1-Iodo-2-phenoxybenzene, 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. Computed Properties of C12H9IO

(1): To 1-iodo-2-phenoxybenzene (2 g, 6.8 mmol)a solution of triethylamine (20 mL) added to phenylacetylene(0.83 g, 8.1 mmol), Pd(PPh3)2Cl2 (95 mg, 135 mumol), CuI (26 mg, 135 mumol).Under argon protection conditions, after 10 hours of reaction,Triethylamine was removed under reduced pressure.The residue was extracted with ethyl acetate (20 mL¡Á3).Then washed twice with water (10 mL) and saturated brine (10 mL).Dry over anhydrous sodium sulfate, filter, and remove the solvent under pressure.The residue was purified by silica gel column chromatography eluting elut1-phenoxy-2-(phenylethynyl)benzene(1.6 g, 88% yield).

The synthetic route of 34883-46-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhongshan University Tumor Cure Center (Zhongshan University Affiliated Tumor Hospital ? Zhongshan University Tumor Institute); Wen Shijun; Huang Peng; Zhu Daqian; Tu Yalin; Luo Bingling; (28 pag.)CN108976248; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com