Month: June 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. 61272-76-2, name is 4-Fluoro-2-iodoaniline, A new synthetic method of this compound is introduced below., Product Details of 61272-76-2

General procedure: An oven-dried flask was charged with o-iodoaniline (13 mmol), the corresponding benzyl bromide(10 mmol), NaHCO3 (20 mmol), and DMF (20 mL). The mixture was stirred at 50 °C under air for 3-4 h.After the completion of the reaction (monitored by TLC), the reaction mixture was cooled to ambienttemperature and 15 mL water was added to the mixture, then extracted by EtOAc for 3 times (3 × 30 mL).The combined extracts were washed with brine, dried over Na2SO4, and the solvent was removed in vacuoto provide a crude product, which was purified by column chromatography on silica gel to afford pure product.

The synthetic route of 61272-76-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Zhengkai; Li, Hongli; Cao, Gangjian; Xu, Jianfeng; Miao, Maozhong; Ren, Hongjun; Synlett; vol. 28; 4; (2017); p. 504 – 508;,
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. 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H9IO2

An ice-cooled solution of 1-iodo-3,5-dimethoxybenzene (8.42 g,31.9 mmol) in DMF (60 mL) was treated under argon atmosphere with freshly distilled POCl3(14 mL, 150 mmol). The mixture was stirred for 30 min at 0 C, then 30 min at roomtemperature and finally heated at 100 C for 5h. The mixture was cooled at room temperatureand was poured with stirring into ice and water (1.5 L). After being stirred for 2h, theresulted suspension was filtered to give a light brown solid. This residue was purified by ashort plug of silica gel using diethyl ether as eluent afforded 1-iodo-3,5-dimethoxybenzaldehyde as a beige solid (5.2 g, 56% yield).1H NMR (300 MHz, CDCl3): delta = 10.1 (s, 1H), 7.13 (d, J = 2.2 Hz, 1H), 6.48 (d, J = 2.2 Hz,1H), 3.89 (s, 3H), 3.86 (s, 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:
Article; Petrignet, Julien; Inack Ngi, Samuel; Abarbri, Mohamed; Thibonnet, Jerome; Tetrahedron Letters; vol. 55; 5; (2014); p. 982 – 984;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

64248-58-4, name is 1,2-Difluoro-4-iodobenzene, 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. COA of Formula: C6H3F2I

Add bis (triphenylphosphine) palladium (II) dichloride (110 mg, 0. 15 mmol), copper (I) iodide (57 mg, 0. 30 mmol), and 3-ethynyl-5-methoxypyridine, (prepared as described in PREPARATION 10), (400 mg, 3. 0 mmol) to a solution of 1, 2-difluoro-4- iodobenzene (0. 43 mL, 3. 6 mmol) in triethylamine (6. 3 mL, 45. 0 mmol) and heat at 60 C for 20 h. Cool to room temperature and concentrate. Purify the residue by silica gel chromatography, eluting with 100 : 0 to 65 : 35 hexanes : ethyl acetate, followed by a second silica gel chromatography, eluting with 100 : 0 to 80 : 20 dichloromethane : ethyl acetate, to give the title compound as a white solid (690 mg, 94%). 1H NMR (300 MHz, CDCl3) 6 3. 89 (s, 3H), 7. 11-7. 21 (m, 1H), 7. 28-7. 40 (m, 3H), 8. 27- 8. 30 (d, J = 2. 9 Hz, 1H), 8. 34-8. 37 (d, J = 1. 6 Hz, 1H), MS (APCI) : m/z = 246 [M+H] +.

The synthetic route of 64248-58-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/94822; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 199850-56-1, 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. 199850-56-1, name is Methyl 2-amino-4-chloro-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

LODINATION of aniline containing compounds: LODINATION was accomplished using a procedure similar to that set forth in the following reference which is herein incorporated by reference in its entirety for all purposes as if fully set forth herein: J. Med. Chem. 2001,44, 6,917-922. The ANTHRANILIC ester in EtOH was added to a mixture of silver sulfate (1 equivalent) and 12 (1 equivalent). The reaction was typically done after 3 hours at room temperature. The reaction was filtered through Celite and concentrated. The residue was taken up in EtOAc and washed with aqueous saturated NAHC03 (3x), water (3x), brine (1X), dried (MGS04), filtered, and concentrated. The crude product (-5 g) was dissolved in MeOH (60-100 mL), NAOH 6 N (25 mL), and water (250 mL). The reactions were typically done after heating at 70-80 C for 4 hours. The reaction mixture was extracted with EtOAc (2x), neutralized with aqueous HCI, filtered to collect the solids, and the solid products were washed with water. The products were dried in vacuo.

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 2-amino-4-chloro-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CHIRON CORPORATION; WO2004/18419; (2004); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 14452-30-3,Some common heterocyclic compound, 14452-30-3, name is 1-(3-Iodophenyl)ethanone, molecular formula is C8H7IO, 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: Acetophenones bearing hydroxy group and or halogens were reacted with substituted benzaldehydes in the presence of 50% (w/v) KOH/H2O using ethanol as a solvent. Purification was done using column chromatography and some chalcones such as those bearing a 4-methoxy group on B-ring can even be recrystallized directly from ethyl acetate-methanol mixture, with acceptable yields ranging from 60-80%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(3-Iodophenyl)ethanone, its application will become more common.

Reference:
Article; Hsieh, Chi-Ting; Hsieh, Tusty-Jiuan; El-Shazly, Mohamed; Chuang, Da-Wei; Tsai, Yi-Hong; Yen, Chiao-Ting; Wu, Shou-Fang; Wu, Yang-Chang; Chang, Fang-Rong; Bioorganic and Medicinal Chemistry Letters; vol. 22; 12; (2012); p. 3912 – 3915;,
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. 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, A new synthetic method of this compound is introduced below., name: Methyl 4-amino-3-iodobenzoate

A combined suspension of methyl 4-amino-3-iodobenzoate (2.0 g, 7.22 mmol), copper (_) iodide (28 mg, 0.14 mmol), bis(triphenylphosphine)palladium(II) dichloride (101 mg, 0.14 mmol), and 1-ethyl-4-ethynylbenzene (1.22 mL, 8.66 mmol) were stirred in toluene and TEA (1/1, 60 mL) at ambient temperature for overnight. The reaction solvent was evaporated under reduced pressure, and the residue was purified by column chromatography with hexane/ethyl acetate (5/1, v/v) to obtain the compound 45 as a white solid (2.02 g, quant. yield): 1H NMR (400 MHz, CDCl3) _ 8.07 (d, J = 2.0 Hz, 1H), 7.78 (dd, J = 8.6, 2.1 Hz, 1H), 7.41 (d, J = 8.2 Hz, 2H), 7.12 (d, J = 8.2 Hz, 2H), 6.64 (d, J = 8.6 Hz, 1H), 4.86 (s, 2H), 3.81 (s, 3H), 2.6 (q, J = 7.6 Hz, 2H), 1.19 (t, J = 7.6 Hz, 3H); 13C NMR (100 MHz, CDCl3) _ 166.6, 151.7, 144.8, 134.1, 131.3, 131.1, 127.9, 119.8, 118.8, 113.1, 107.1, 95.2, 84.1, 51.6, 28.7, 15.2.

The synthetic route of 19718-49-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM; DALBY, Kevin N.; EDUPUGANTI, Ramakrishna; TALIAFERRO, Juliana; LEE, Juhyeon; (0 pag.)WO2018/160967; (2018); 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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), A new synthetic method of this compound is introduced below., Safety of 1,3-Diiodopropane(stabilized with Copper chip)

Diiodopropane (0.295 g, 1.00 mmol, 5.0 eq) and potassium carbonate (0.028 g, 0.20 mmol, 1.0 eq) were added to a solution of the phenol 33 (0.100 g, 0.020 mmol, 1.0 eq) in dry acetone (5 mL). The reaction mixture was heated at 60C for 6 hours when LC/MS showed complete reaction. The reaction mixture was concentrated to dryness under reduced pressure and the residue was purified by flash chromatography (silica gel, 75/25 v/v n-hexane/EtOAc to 50/50 v/v n-hexane/EtOAc) to afford the product as a colourless oil (0.074 g, 56%). LC/MS (3.853 min (ES+)), m/z: 669.0 [M+H]+. 1H NMR (400 MHz, CDC13) delta 7.26 (s, 1H), 6.90 (s, 1H), 6.68 (s, 1H), 6.24 (d, 1H, / = 15.3 Hz), 5.87 (d, 1H, / = 8.9 Hz), 5.78 (m, 1H), 5.53 (m, 1H), 5.12 (m, 2H), 4.65 (m, 2H), 4.41 (m, 1H), 4.11 (m, 1H), 3.93 (s, 3H), 3.81 (m, 1H), 3.40 (t, 2H, / = 6.7 Hz), 3.05 (dd, 1H, / = 16.3, 10.1 Hz), 2.57 (m, 1H), 2.34 (m, 2H), 1.84 (d, 3H, / = 6.6 Hz), 0.92 (s, 9H), 0.28 (s, 3H), 0.26 (s, 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; MEDIMMUNE LIMITED; LLOYD, Christopher O.; MARWOOD, Rose; HOWARD, Philip; HARPER, III, John W.; HOLLINGSWORTH, Robert; KAMAL, Adeela; DIMASI, Nazzareno; GAO, Changshou; TOADER, Dorin; WANG, Fengjiang; GINGIPALLI, Lakshmaiah; WO2015/155345; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 20555-91-3, 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. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: An appropriate phenylacetamide (0.12 mmol, 1 equiv), an appropriate iodo compound (0.48 mmol, 4 equiv), Pd(OAc)2 (2.7 mg, 10 mol%), and AgOAc (50 mg, 0.3 mmol, 2.5 equiv) in anhydrous toluene (3 mL) was heated at 110 C for 24 h under a nitrogen atmosphere. After the reaction period, the solvent was evaporated in vacuo to afford a crude reaction mixture. Purification of the crude reaction mixture by column chromatography furnished the corresponding arylated products 4a-q/7a-f (bis arylation products), 3o,r/6a,b/8e,f/9a,b (mono arylation products) (see corresponding Tables/Schemes for specific examples and reaction conditions).

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, 1,2-Dichloro-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Bisht, Narendra; Babu, Srinivasarao Arulananda; Tetrahedron; vol. 72; 39; (2016); p. 5886 – 5897;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 31599-61-8, A common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, molecular formula is C8H9I, 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.

14 Typical procedure for the preparation of 4,5-disubstituted-1,2,3-(NH)-triazoles (synthesis of 3a): A round-bottom sidearm flask (10 mL) containing PdCl2(PPh3)2 (0.015 mmol) was subjected to the Schlenk-line procedures of evacuation and purging of CO for three cycles. Iodobenzene and 4 equiv Et3N (1.2 mmol) were successively added, and the mixture was stirred at room temperature for 10 min, then 1-hexyne (0.45 mmol) was added, continuously stirred at room temperature for 14 h. Then NaN3 (35.1 mg, 0.54 mmol) and 1 mL DMSO were added to the mixture and the reaction continued at 45 C for 36 h. Following, to the reaction mixture was added water (2 mL), 20% HCl solution (1 mL) and extracted with ether (3 * 10 mL). The combined organic phases were washed with brine (2 * 5 mL), dried over anhydrous MgSO4 and concentrated in vacuo. The residue was subjected to flash column chromatography with hexanes/EtOAc (5/1) as eluent to obtain the desired 3a (56.33 mg, 82% yield). All products gave satisfactory spectroscopic and analytical data.

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, Na; Wang, Dong; Li, Jihui; Shi, Weilin; Li, Chao; Chen, Baohua; Tetrahedron Letters; vol. 52; 9; (2011); p. 980 – 982;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 52807-27-9,Some common heterocyclic compound, 52807-27-9, name is 4-Chloro-2-iodoanisole, molecular formula is C7H6ClIO, 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.

Add to a solution of 4-chloro-2-iodoanisole (10 g, 37.24 mmol) in 1,4-dioxane (50 mL) is 2-thiopheneboronic acid (5.71 g, 44.66 mmol), (2-dicyclohexylphosphino)-2′- methylbiphenyl (2.71 g, 7.44 mmol), palladium acetate (0.418 g, 1.86 mmol) and potassium fluoride (6.49 g, 111.7 mmol). Stir at 95 C for 18 h, cool to room temperature, filter through a filtering agent and wash with ethyl acetate (400 mL). Wash organic layer with water (3 x 100 mL), saturated aqueous sodium chloride (1 x 100 mL), dry over sodium sulfate, filter, concentrate and purify (HPLC, eluting with hexanes) to give the titled compound as an oil (5.4g). HRMS m/z Calculated: 225.0141; Found: 225.0132

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

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/100301; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com