Month: April 2021

Adding a certain compound to certain chemical reactions, such as: 25245-35-6, name is 2-Iodo-1,4-dimethoxybenzene, 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 25245-35-6, SDS of cas: 25245-35-6

To a stirred solution of 2-iodo-1,4-dimethoxybenzene (4b, 264 mg; 1.0 mmol) and tert-butyl alcohol (0.25 mL) in glacialacetic acid (0.2 mL) at 0 C was added dropwise over 2 min concentrated H2SO4 (0.3mL). The reaction was stirred at 0 C for 2 h and then allowed to warm to roomtemperature and stirred overnight. Work up consisted of partitioning the reaction mixturebetween water and ethyl acetate, followed by washing the organic layer with dil. aqNaHCO3, water and drying (Na2SO4). Preparative TLC (hexane-CH2Cl2, 1:1) producedrecovered starting material (67 mg) and the product (148 mg; 46%; 62% based onrecovered starting material). Mp 79-82 C (Lit: 81-83 C [3]). 1H-NMR (CDCl3, 500MHz): 1.35 (s, 9H, But), 3.79 (s, 3H, OCH3), 3.83 (s, 3H, OCH3), 6.81 (s, 1H), 7.20 (s,1H).

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-Iodo-1,4-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kempton, Robert J.; Kidd-Kautz, Taylor A.; Laurenceau, Soizic; Paula, Stefan; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 971 – 975;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 6940-76-7, These common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, 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.

Sodium hydride (1.96 g, 49.337 mmol, 60% suspension in mineral oil) was treated with DMF (60 mL), followed by 6-nitroindole (6) (2.0 g, 12.334 mmol) in DMF (20 mL) over a period of 5 min at 0 C. After stirring for 15 min, the solution was treated with 1-chloro-3-iodopropane (3.9 mL, 37.002 mmol), the reaction was brought to room temperature and stirred for 3 h. The reaction was quenched with saturated brine (80 mL), water (80 mL) and cooled to 0 C. The solid was filtered off, washed with water (50-75 mL) and dried to obtain the crude product. The crude product was recrystallised from hot toluene (10 mL)/hexanes (5 mL) to obtain compound 148 (2.637 g, 90%) as solid. mp 85-87 C.; 1H-NMR (CDCl3) delta 2.28-2.36 (m, 2H), 3.46 (t, 2H, J=5.7 Hz), 4.45 (t, 2H, J=6.6 Hz), 6.62 (d, 1H, J=2.7 Hz), 7.43 (d, 1H, J=3.0 Hz), 7.66 (d, 1H, J=8.7 Hz), 8.02 (dd, 1H, J=1.8, 7.9 Hz), 8.36 (d, 1H, J=0.9 Hz).

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Maddaford, Shawn; Ramnauth, Jailall; Rakhit, Suman; Patman, Joanne; Renton, Paul; Annedi, Subhash C.; US2006/258721; (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. 628-21-7, name is 1,4-Diiodobutane, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

General procedure: A suspension of alkenyl- or aryl-dithiol(1.0 mmol), triethylamine (2.0 mmol), LR (0.44g, 1.0 mmol) or FcLR (0.56 g, 1.0 mmol) and dihaloalkane(1.0 mmol) in dry THF (60 mL) was stirred under N2 gas atmosphere at ambient temperature for 24 h leadingto a reddish yellow or pale-yellow suspension. Upon filtering to remove insoluble solid the filtrate was driedunder reduced pressure. The residue was dissolved in dichloromethane (ca. 2 mL) and was loaded onto a silicagel column (dichloromethane as eluent) to give the macrocycles. Another unexpected nine-membered ring 4was also obtained in respective 25% and 30% yields in the cases of 5 and 9. Two diastereomers wereseparated completely in the cases of 10 and 12.

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; Hua, Guoxiong; Cordes, David B.; Slawin, Alexandra M. Z.; Woollins, J. Derek; Synlett; vol. 29; 11; (2018); p. 1496 – 1501;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 915095-86-2, name is (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, molecular formula is C13H7ClFIO, 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. Quality Control of (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone

(5-iodo-2-chlorophenyl) (4-fluorophenyl) methanone (18.03 g, 50 mmol) was added DMS0 (80 mL) Ice bath slowly add lithium ethoxide (3.128,1.2 called), After adding 0 ¡ã (below the stirring reaction 311, hole (after the reaction is completed, add water (240mL) slowly under ice bath, Stirring crystallization lh, Filter, The filter cake was washed with water (200 mL) Beat with ethanol (50 mL) Filter, Dried to give 15.99 g of a pale yellow solid of compound lib, yield: 82.7percent, purity: 99.44percent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 915095-86-2, its application will become more common.

Reference:
Patent; Shanghai Pharmaceutical Industry Institute; China Pharmaceutical Industry Zongyuan; Ma Shuai; Zhou Weicheng; (7 pag.)CN106928040; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 105202-02-6, name is 2-Iodo-5-(trifluoromethyl)aniline, 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 105202-02-6, Product Details of 105202-02-6

To a solution of compound 53 (620 mg, 2.16 mmol) in DMF (5 mL) was added phenylacetylene (331 mg, 356 muL, 3.24 mmol), PdCI2(PPh3)2 (76 mg, 0.108 mmol), Cul (25 mg, 0.131 mmol) and Et3N (656 mg, 903 muL, 6.48 mmol) at 23 C. The reaction mixture was stirred for 6 h at 23 C before it was quenched with a saturated solution of NH4CI (10 mL) and diluted with EtOAc (50 mL). The layers were separated, and the organic layer was extracted with H20 (3 x 10 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexanes:EtOAc 5: 1 ) to give compound 54 (518 mg, 92%) as pale yellow solid. (0472) [00362] 1 H NMR (400 MHz, CDCI3) delta = 7.56 (m, 2H), 7.47 (dd, J = 8.5, 0.8 Hz, 1 H), 7.42 – 7.38 (m, 3H), 6.98 – 6.96 (m, 2H), 4.48 (brs, 2H); 13C NMR (101 MHz, CDCI3) delta = 147.8, 132.5, 131 .6, 131 .5 (q, J = 32.2 Hz), 128.7, 128.5, 124.0 (q, J = 272.3 Hz), 122.6, 1 14.3 (q, J = 3.8 Hz), 1 1 1 .2, 1 10.7 (q, J = 4.0 Hz), 96.5, 84.6; 19F NMR (376 MHz, CDCI3) delta = -63.13. m/z (ESI) 262.1 [M+H+].

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; THE GOVERNING COUNCIL OF THE UNIVERSITY OF TORONTO; GREIG, Iain; ZANDA, Matteo; TSENG, Chih-Chung; ROSS, Ruth; (134 pag.)WO2016/29310; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 54413-93-3, These common heterocyclic compound, 54413-93-3, name is 2-Iodo-5-methoxybenzoic 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.

General procedure: In a 10 mL glass tube 2-iodobenzoic acid (1.0 mmol), acetamidine hydrochloride (1.2 mmol), CuCl2 (0.1 mmol), L2 (0.1 mmol), and NaOH (4.0 equiv.) and 3.0 mL water were placed. The vessel was then sealed with a septum and placed into the microwave cavity. Initial microwave irradiation of 120 W by using a CEM Discover microwave synthesizer was used at the room temperature for 20 min. The reaction mixture was stirred continuously during the reaction. After completion of the reaction, the solvent was removed in vacuo. The residue was purified by silica gel column chromatography to afford the corresponding product. All the products were confirmed by NMR and MS spectroscopic analysis.

The synthetic route of 54413-93-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ke, Fang; Liu, Caiqin; Zhang, Peng; Xu, Jianhua; Chen, Xiaole; Synthetic Communications; vol. 48; 24; (2018); p. 3089 – 3098;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 6293-83-0,Some common heterocyclic compound, 6293-83-0, name is 2-Iodo-4-nitroaniline, molecular formula is C6H5IN2O2, 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 11 Preparation of 2-Iodo-p-phenylenediamine A mixture of concentrated hydrochloric acid (150 ml) and 2-iodo-4-nitroaniline (30.0 g) is stirred and warmed to 45¡ã-50¡ã C. A solution of stannous chloride dihydrate (90.0 g) in concentrated hydrochloric acid (110 ml) is added while maintaining the reaction temperature at 65¡ã-70¡ã C. After the addition is completed, the mixture is cooled in an ice bath and 50percent sodium hydroxide (250 ml) is added slowly. The mixture is filtered and the isolated damp solid is stirred in 600 ml water at reflux. The solution is decolorized with charcoal, filtered and cooled to afford 5.55 g of title compound, m.p. 95¡ã-99¡ã C.

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

Reference:
Patent; American Cyanamid Company; US4239708; (1980); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, 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 328-73-4, name: 1-Iodo-3,5-bis(trifluoromethyl)benzene

EXAMPLE 7 Preparation of 2-(3,5-bis-(trifluoromethyl)-phenyl)-indene 20 ml of triethylamine, 2.2 g (20 mmole) of indene, 6.8 g (20 mmole) of 1-iodo-3,5-bis(trifluoromethyl)-benzene and 0.134 g (0.6 mmole) and 0.134 g (0.6 mmole) of Pd(OAc)2 were stirred under relux for 12 h. After it all triethylamine was removed under reduced pressure. The residue was treated with the mixture 50 ml of water and 50 ml of diethyl ether. Etherial layer was separated, washed twice with water, filtered and dried over Na2SO4. Ether was removed and some 20 ml of pentane were added to the reaction mixture, it was cooled down to -20¡ã C. and product was crystallized as dark needle crystals, which were filtered, washed with small portion of cold pentane and dried in vacuum. The yield of product was 32percent. 1H NMR (CDCl3): 8.06 (bs, 2H); 7.80 (bs, 1H); 7.58-7.48 (m, 3H); 7.42-7.32 (m, 2H); 3.88 (s, 2H).

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, 1-Iodo-3,5-bis(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Montell Technology Company bv; US6271411; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

401-81-0, name is 1-Iodo-3-(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. category: iodides-buliding-blocks

General procedure: A 50mL round-bottomed flask equipped with a gas inlet tube, a reflux condenser, and a magnetic stirring bar was charged with MCM-41-S-PdCl2 (173mg, 0.05 mmol Pd), aryl halide (5.0 mmol) and HCOONa (7.5 mmol). The flask was flushed with carbon monoxide. DMF (5 mL) was added by syringe and a slow stream of CO was passed into the suspension. The mixture was vigorously stirred at 100-110C for 4-24h, cooled to room temperature, and diluted with diethyl ether (50 mL). The palladium catalyst was separated from the mixture by filtration, washed with distilled water (2¡Á10 mL), ethanol (2¡Á10 mL) and ether (2¡Á10 mL) and reused in the next run. The ethereal solution was washed with water (3¡Á20mL) and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (hexane-ethyl acetate=10:1). (0008) All formylation products were characterized by comparison of their spectra and physical data with authentic samples. IR spectra were determined on a Perkin-Elmer 683 instrument. 1H NMR (400MHz) and 13C NMR (100MHz) spectra were recorded on a Bruker Avance 400MHz spectrometer with TMS as an internal standard and CDCl3 as solvent.

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hao, Wenyan; Ding, Guodong; Cai, Mingzhong; Catalysis Communications; vol. 51; (2014); p. 53 – 57;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3718-88-5, 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 3718-88-5 as follows.

A suspension of 3-iodobenzylamine hydrochloride (4.95g, 18.4 mmol) in dichloromethane (100 ml) was treated with triethylamine (3.1 ml, 22 mmol) and di-t-butyl dicarbonate (4.40g, 20 mmol) and the resulting solution left to stir at room temperature under a nitrogen atmosphere for 1.5 hours. The reaction mixture was washed with 2M hydrochloric acid (30 ml), water (30 ml), dried (sodium sulfate), and the solvent removed in vacuo to give the title compound as a colourless solid (6.43g). 1HNMR (400 MHz, CDCl3) delta: 1.46 (s, 9H), 4.21-4.30 (m, 2H), 4.79-4.89 (bs, 1H), 7.06 (dd, 1H), 7.25 (d, 1H), 7.60 (d, 1H), 7.63 (s, 1H) ppm. MS (electrospray) m/z 332 [M-H]-, 356 [M+Na]+

According to the analysis of related databases, 3718-88-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Brown, Alan Daniel; Bunnage, Mark Edward; Glossop, Paul Alan; James, Kim; Lane, Charlotte Alice Louise; Lewthwaite, Russel Andrew; Moses, Ian Brian; Price, David Anthony; Thomson, Nicholas Murray; US2005/182091; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com