Month: September 2021

Application of 354574-31-5, 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. 354574-31-5, name is 2-Iodo-6-methoxyaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 2-iodo-6-methoxybenzenamine 10 (2.49 g, 10 mmol), methyl5-formylpentanoate 11 (1.59 g, 11 mmol) and DABCO (6.60 g, 30 mmol) in dry DMF (45 mL) was degassed for 20 min. Pd(OAc)2 (230 mg, 1 mmol) was added to the reaction,and the resulting mixture was heated at 85C under argon atmosphere overnight. The reaction mixture was cooled to room temperature and diluted with water followed by extraction with EtOAc.The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentratedin vacuo. The residue was purified by FCC (PE-Acetone, 8:1) to give 12 (1.43 g, 58%) as white foam.

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

Reference:
Article; Wang, Bin; Qin, Hua; Zhang, Fengying; Jia, Yanxing; Tetrahedron Letters; vol. 55; 9; (2014); p. 1561 – 1563;,
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. 455-13-0, name is 4-Iodobenzotrifluoride, A new synthetic method of this compound is introduced below., Quality Control of 4-Iodobenzotrifluoride

General procedure: A sealed 10 mL glass tube containing aryl halide (1 mmol), CS2(0.5 mmol) and [DBUH]+[OAc]- (1 mL) was placed in the cavity of a microwave reactor and irradiated for 5-60 min at 100-120 C and power 150 W. After cooling to room temperature, the reaction mixture was extracted with Et2O (3 × 5 mL) and the [DBUH]+[OAc]-was separated from the product. The organic layers were combined and the solvent removed under reduced pressure to provide the crude product, which was further purified by column chromatography on silica gel using petroleum ether/EtOAc as the eluent. The recovered [DBUH]+[OAc]- was washed with diethyl ether and could be reused in the next reaction. All of the products are known compounds and their characterisation data were compared and are consistent with literature reports.

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; Zhou, Yongsheng; Journal of Chemical Research; vol. 40; 5; (2016); p. 305 – 307;,
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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H4ClIO2

Example 494r-Chloro-3f-[[(2-tricyclo[3.3.1.13’7]dec-l-ylethyl)ammo]carbonyl]-[l,l’-biphenyl]-2-carboxylic acid0 Cla) 2-Chloro-5-iodo-benzoic acid, 1,1-dimethylethyl esterN,N-Dimethylformamide (1 drop) and oxalyl chloride (4.8 mL) were added to a stirredsolution of 2-chloro-5-iodobenzoic acid (5 g) in dichloromethane (20 mL) at 0 C. Thereaction was allowed to warm to room temperature, stirred under nitrogen for 2 hours, andthen evaporated to dryness. The residue was dissolved in tetrahydrofuran (20 mL) andcooled to 0 C. Potassium tert-butoxide (22 mL, 1 M solution in tetrahydrofuran) wasadded over 10 minutes. The reaction was allowed to warm to room temperature and stirredunder nitrogen for 2 hours then poured into saturated aqueous sodium bicarbonate (50 mL).The layers were separated and the aqueous was extracted with diethyl ether (50 mL). Thecombined organics were dried, filtered and evaporated to afford the sub-title compound asan oil (5.7 g).JH NMR (400 MHz, d6-DMSO) 5 7.99 (1H, d), 7.87 (1H, dd), 7.34 (1H, d), 1.54 (9H, s).

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 19094-56-5.

Reference:
Patent; ASTRAZENECA AB; WO2006/25783; (2006); 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., Application In Synthesis of 5-Iodobenzo[d][1,3]dioxole

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

Synthetic Route of 624-75-9, 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. 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.

To a ice cooled stirred solution of ((benzyloxy)carbonyl)-phenylalanine (19) (0.5 g, 1.670 mmol) and TEA (0.233 mL, 1.670 mmol) in DMF (5 mL) was added 2-iodoacetonitrile (0.121 mL, 1.670 mmol) drop-wise and the resulting solution was stirred at room temperature for 12 h. The progress of the reaction was monitored by TLC. After completion, the reaction mixture was diluted with water (20 mL) and extracted with ethyl acetate (2 x 25 mL). Combined organic layer was washed with water (50 mL), saturated brine solution (50 mL) and dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure to afford brown gummy liquid of the crude product. The crude compound was purified by silica-gel flash column chromatography (eluted with ethyl-acetate/pet-ether = 2/10) to afford Cyanomethyl ((benzyloxy)carbonyl)phenylalaninate (1f) (0.5 g, 88%) as off-white solid. 1H NMR (300 MHz, DMSO-d6): delta 7.19-7.38 (m, 11H), 5.02 (s, 2H), 4.96 (d, 2H), 4.33-4.41 (m, 1H), 2.87-3.10 (m, 2H). 13C NMR (75 MHz, DMSO-d6): delta 171.4, 156.3, 136.4, 137.3, 137.2, 129.6, 128.8, 128.7, 128.2, 128.0, 127.1, 116.1, 65.9, 55.6, 49.9, 36.5 MS (ESI): 356.2 as [M+H2O] in +Ve mode and as 338.2 [M-1] in -Ve mode.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Iodoacetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Karmakar, Ananta; Basha, Mushkin; Venkatesh Babu; Botlagunta, Murali; Malik, Noormohamed Abdul; Rampulla, Richard; Mathur, Arvind; Gupta, Arun Kumar; Tetrahedron Letters; (2018); p. 4267 – 4271;,
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. 610-97-9, name is Methyl 2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: Methyl 2-iodobenzoate

General procedure: Propargylic precursors 2a-2j were prepared by Sonogashira reaction of aryl halides with appropriate terminal propargyl alcohols by following a literature procedure [9]. Among these propargyl alcohols 2d-2f are new. The general procedure for the synthesis of these compounds is given below. Compound 2a: To a stirred solution of aryl iodide (2.62 g, 10 mmol), PdCl2 (0.018 g, 0.1 mmol), PPh3 (0.053 g, 0.2 mmol) and CuI (0.039 g, 0.2 mmol) in triethylamine (15 mL) was added propargyl alcohol (1.07 g, 20 mmol) at rt (25oC). The contents were stirred at reflux for 10 h. After all the starting material was consumed (TLC), the reaction mixture was filtered and the solvent removed by vacuum. The product 2a was purified by column chromatography using silica gel with ethyl acetate/hexane mixture (1:4) as the eluent. yield: 1.67 g (88%). The spectral data are in accordance with the literature report [10]. Propargyl alcohols 2b-2fwere prepared using same molar quantities. Among these compounds 2a-2c are known and 2d-2f are new.

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 610-97-9.

Reference:
Article; Gangadhararao; Kotikalapudi, Ramesh; Reddy, M. Nagarjuna; Swamy Kumara; Beilstein Journal of Organic Chemistry; vol. 10; (2014); p. 996 – 1005;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, 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 90347-66-3, Product Details of 90347-66-3

A mixture of methyl 3-iodo-4-methylbenzoate (2 g, 7.2 mmol, 1.0 eq) and CuCN (774 mg, 8.6 mmol, 1.2 eq) in NMP (20 mL) was stirred at 200 C wiht microwave for 1 h. Then the mixture was poured into water (50 mL), extracted with EtOAc (50 mL x3). The combined organic layers were washed with brine (20 mL), dried over anhydrous Na2S04 and concentrated. The residue was purified on silica gel column (PE/EtOAc = 5/1) to afford methyl 3-cyano-4-methylbenzoate as a white solid (1.2 g, 95%>).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 3-iodo-4-methylbenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; LIFESCI PHARMACEUTICALS, INC.; MCDONALD, Andrew; WO2015/103317; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 624-76-0, The chemical industry reduces the impact on the environment during synthesis 624-76-0, name is 2-Iodoethanol, I believe this compound will play a more active role in future production and life.

General procedure: A mixture of compound 1 (1 mmol) in acetonitrile (30 mL) and functionalized alkyl halides(1.3 mmol) was irradiated by ultrasound irradiation. The reaction was processed as described above togive the same ionic liquids 2-7.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Iodoethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Rezki, Nadjet; Al-Sodies, Salsabeel A.; Shreaz, Sheikh; Shiekh, Rayees Ahmad; Messali, Mouslim; Raja, Vaseem; Aouad, Mohamed R.; Molecules; vol. 22; 11; (2017);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 6828-35-9, 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. 6828-35-9 name is 5-Chloro-2-iodoaniline, 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.

5-Chloro-2-((trimethylsilyl)ethynyl)aniline To a solution of 5-chloro-2-iodoaniline (1.50 g, 5.92 mmol) and ethynyltrimethylsilane (1.25 ml, 8.88 mmol) in Et3N (20 ml) was added CuI (5.6 mg, 0.030 mmol) and Pd(PPh3)2Cl2 (21 mg, 0.030 mmol) and the mixture was stirred at room temperature for 5 hours. Celite was added and the suspension was filtered, rinsed with EtOAc. The filtrate was concentrated in vacuo to yield Intermediate 1 as a yellow oil (1.32 g, 100%). 1H NMR (CHLOROFORM-d) delta: 7.20 (d, J=8.2 Hz, 1H), 6.69 (d, J=1.8 Hz, 1H), 6.63 (dd, J=8.2, 2.1 Hz, 1H), 4.30 (br. s., 2H), 0.27 (s, 9H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Chloro-2-iodoaniline, and friends who are interested can also refer to it.

Reference:
Patent; ALLERGAN, INC.; YUAN, HAIQING; BEARD, RICHARD L.; LIU, XIAOXIA; DONELLO, JOHN E.; VISWANATH, VEENA; GARST, MICHAEL E.; US2013/231338; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

5326-47-6, These common heterocyclic compound, 5326-47-6, name is 2-Amino-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.

Concentrated H2SO4 (3.7 mL) was added dropwise at 20 C under argon atmosphere to a stirred solution of 5-iodoanthranilic acid (5.0 g, 19 mmol) in MeOH (20 mL), and the mixture was refluxed for 7 h. The mixture was then concentrated in vacuo to the volume of 10 mL, poured into a vigorously stirred saturated solution of NaHCO3 (80 mL), and extracted with EtOAc. The organic layer was washed with a brine solution, dried over Na2SO4, and concentrated in vacuo; the residue was purified by chromatography on SiO2 (eluent was benzene). Ester 6 (3.68 g) was isolated as yellow crystals, m.p. 80-82 C (LP). 1H NMR (CDCl3), delta: 3.87 (s, 3 H, MeO); 5.76 (br.s, 2 H, H2N); 6.46 (d, 1 H, HC(3), J = 8.7 Hz); 7.48 (dd, 1 H, HC(4), J = 8.7 Hz, J = 2.2 Hz); 8.14 (d, 1 H, 2 HC(6), J = 2.2 Hz); which is similar to that reported previously.24

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 5326-47-6.

Reference:
Article; Lozanova; Stepanov; Mel?nik; Zlokazov; Veselovsky; Russian Chemical Bulletin; vol. 68; 1; (2019); p. 64 – 67; Izv. Akad. Nauk, Ser. Khim.; 1; (2019); p. 64 – 67,4;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com