Author: Jessica.F

Application of 61272-76-2, These common heterocyclic compound, 61272-76-2, name is 4-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.

General procedure: to ortho iodoaniline,1(a?q) (0.10 mmol), in dioxane (5 mL) was added PdCl2 (5 mol percent), A-taphos(10 mol percent). The solution was purged with nitrogen and stirred at roomtemperature for 10 min and aldehyde (2a?q) (0.16 mmol), CH3COOCs(0.20 mmol), were added. The reaction mixture was again purged withnitrogen and heated in the microwave at 120 C for 30?40 min. Reaction wasmonitored by TLC. After the completion, reaction mixture was cooled to roomtemperature and water was added to the reaction mixture. It was thenextracted with ethyl acetate (25 mL 2) and the separated organic layer wasdried over anhydrous Na2SO4. The organic layer was filtered and concentratedunder vacuum, and the residue was purified by flash column chromatographyon silica gel.

Statistics shows that 4-Fluoro-2-iodoaniline is playing an increasingly important role. we look forward to future research findings about 61272-76-2.

Reference:
Article; Karuvalam, Ranjith P.; Haridas, Karickal R.; Sajith, Ayyiliath M.; Muralidharan, Arayambath; Tetrahedron Letters; vol. 54; 37; (2013); p. 5126 – 5129;,
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Synthetic Route of 13194-68-8, The chemical industry reduces the impact on the environment during synthesis 13194-68-8, name is 4-Iodo-2-methylaniline, I believe this compound will play a more active role in future production and life.

(b) Preparation of 5-Bromo-3,4-difluoro-2-(4-iodo-2-methyl-phenylamino)-benzoic acid To a stirred solution comprised of 1.88 g (0.00791 mol) of 2-amino-5-iodotoluene in 10 mL of tetrahydrofuran at -78 C. was added 6 mL (0.012 mol) of a 2.0 M lithium diisopropylamide in tetrahydrofuran/heptane/ethylbenzene (Aldrich) solution. The resulting green suspension was stirred vigorously for 10 minutes, after which time a solution of 1.00 g (0.00392 mol) of 5-bromo-2,3,4-trifluorobenzoic acid in 15 mL of tetrahydrofuran was added. The cold bath was subsequently removed, and the reaction mixture stirred for 18 hours. The mixture was concentrated, and the concentrate was treated with 100 mL of dilute (10%) aqueous hydrochloric acid. The resulting suspension was extracted with ether (2*150 mL), and the combined organic extractions were dried (MgSO4) and concentrated in vacuo to give an orange solid. The solid was triturated with boiling dichloromethane, cooled to ambient temperature, and collected by filtration. The solid was rinsed with dichloromethane, and dried in the vacuum-oven (80 C.) to afford 1.39 g (76%) of a yellow-green powder, mp 259.5-262 C.; 1H NMR (400 MHz, DMSO): delta 9.03 (s, 1H), 7.99 (dd, 1H, J=7.5, 1.9 Hz), 7.57 (dd, 1H, J=1.5 Hz), 7.42 (dd, 1H, J=8.4, 1.9 Hz), 6.70 (dd, 1H, J=8.4, 6.0 Hz), 2.24 (s, 3H); 19F NMR (376 MHz, DMSO): delta -123.40 to -123.47 (m); -139.00 to -139.14 (m); IR (KBr) 1667 (C=O stretch)cm-1; MS (CI) M+1=469.

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, 4-Iodo-2-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Warner-Lambert Company; US6251943; (2001); B1;,
Iodide – Wikipedia,
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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. 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 26670-89-3

Compound 1 (3 g, 10.10 mmol, 1 eq) in THF (30 mL) was placed into 250 ml round bottom flask. The reaction solution was cooled to -65 C. under a nitrogen atmosphere. n-BuLi (2.2 M, 5.05 mL, 1.1 eq) to the cooled solution was slowly added dropwise, the mixture was stirred for 1 h at the same temperature. TRIMETHYL BORATE (1.26 g, 12.12 mmol, 1.37 mL, 1.2 eq) were added dropwise to the above solution at the same temperature. The mixture was stirred at -65 OC for 1 h. Then cool bath was removed and the mixture was stirred at -65?10 C. for 16 h. The mixture was acidified by dropwise addition of HCl solution (2 M, 5 mL) to the reaction solution, which was stirred for 1.5 hour. The mixture were concentrated in vacuum to afford a residue. The residue was purified by reverse-MPLC (FA condition, A: water, B: MeCN, 40% B). The fraction were concentrated to remove solvent, and aqueous phase was extracted with ethyl acetate (50 mL*3). The combined organic layers were washed with brine (50 mL), dried over sodium sulfate, filtered and the filtrate was concentrated in vacuum to give Compound 2 (1.3 g, 6.05 mmol, 59% yield) as white solid. 1H NMR (400 MHz, DMSO-d6) delta=8.15 (s, 0.5H), 7.95 (s, 0.3H), 7.93 (s, 1H), 7.73 (d, J=7.5 Hz, 1H), 7.66 (d, J=7.5 Hz, 0.3H), 7.37 (d, J=7.5 Hz, 1H), 7.32 (d, J=7.6 Hz, 0.3H), 2.37 (s, 3H), 2.34 (s, 0.9H).

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; 1ST Biotherapeutics, Inc.; LEE, Jinhwa; KIM, Jae Eun; JO, Suyeon; LEE, Gwibin; LIM, Keonseung; PARK, A Yeong; KIM, Misoon; JUNG, Gyooseung; LIM, Seung Mook; LEE, Minwoo; YANG, Heekyoung; KIM, Hyonam; KIM, Hyeongjun; LI, Wanjun; FAN, Mingzhu; (82 pag.)US2019/100500; (2019); A1;,
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Related Products of 76801-93-9, 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. 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(b) (+)-5-Acetamido-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide The dextrorotatory compound was prepared from (+)-5-amino-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide (21 g) by acetylation and a subsequent hydrolysis at pH 10-11 in a similar manner to that described in C(a) above. Finally the product was recrystallized from water. Yield: 13.6 g (61%) [alpha]546 =+4.0; [alpha]578 =+3.8 (c=4.5; DMF:H2 O=2:8). Melting Point: 285-289 dec. Analysis–Found: C, 25.80; H, 2.50; I, 50.6; N, 5.71. Calc. for C16 H20 I3 N3 O7: C, 25.72; H, 2.70; I, 50.95; N, 5.62.

The synthetic route of 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nyegaard & Co. A/S; US4250113; (1981); A;,
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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. 19821-80-8, name is 1,3-Dibromo-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 19821-80-8

Synthesis Example 2 (Synthesis of 2,6-Dimesityliodobenzene) A solvent of 200 mL of THF was added to 6.0 g (250 mmol) of magnesium (Wako Pure Chemical Industries, Ltd.) and a trace amount of iodine. In 100 mL of THF was dissolved 34 mL (225 mmol) of bromomesitylene (Wako Pure Chemical Industries, Ltd.). The solution was added dropwise to the above magnesium/THF slurry at room temperature in 2 hours. After the completion of the dropping, the solution was refluxed for 2 hours, and then cooled to room temperature. In 50 mL of THF was dissolved 23 g (64 mmol) of 1,3-dibromoiodobenzene. The solution was added dropwise to the above Grignard solution at room temperature in 1 hour. The reaction liquid was refluxed for 3 hours, and then cooled to 0C. A solution of 25 g (100 mmol) of iodine in 50 mL of THF was added dropwise to the reaction mixture, followed by warming to room temperature. The reaction mixture was washed with a saturated aqueous solution of sodium sulfite, and then extracted three times with diethyl ether. The ether layers were mixed, then washed with water and saturated brine, and then dried with magnesium sulfate. The solvent was removed under reduced pressure, and the byproduct was then removed under reduced pressure. The residue was recrystallized from methanol, giving 19.7 g of white solid of 2,6-dimesityliodobenzene (70% in yield). It was confirmed that the product was 2,6-dimesityliodobenzene by 1H-NMR. 1H-NMR (400MHz, CDCl3) 1.98 (s, 12H, o-CH3), 2.35 (s, 6H, p-CH3), 6.96 [s, 4H, m-H (Mes)], 7.08 [d, J = 7.6 Hz, 2H, m-H (Ph)], 7.46 [t, J = 7.6 Hz, 1H, p-H (Ph)].

The synthetic route of 19821-80-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Otsuka Chemical Holdings Co., Ltd.; EP2133357; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic acid, 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. Quality Control of 2-Iodo-4,5-dimethoxybenzoic acid

General procedure: DMF (2 drops) and oxalyl chloride (180 muL, 2.12 mmol) were added to a suspension of 4-chloro-2-iodobenzoic acid (0.400 g, 1.42mmol) in toluene (5 mL). After the acid had dissolved and evolution of gas had ceased, the mixture was concentrated under vacuum to afford the crude acyl chloride, which was used without further purification.To a soln of this crude acyl chloride in CH2Cl2 (6 mL) was added a soln of Et3N (592 muL, 4.25 mmol) and aniline (129 muL,1.42 mmol) in CH2Cl2 (6 mL). The mixture was stirred for 1 h and then sat. aq NH4Cl soln (5 mL) was added. The aq layer was extracted with CH2Cl2 (3 × 5 mL) and the combined organic layers dried (Na2SO4) and evaporated. The crude residue was purified by flash chromatography (hexanes-EtOAc, 90:10 to 85:15), to afford 5e (400 mg, 79%) as a white solid.

The synthetic route of 61203-48-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Madich, Youssef; Denis, J.Gabriel; Ortega, Aitor; Martinez, Claudio; Matrane, Abdellatif; Belachemi, Larbi; De Lera, Angel R.; Alvarez, Rosana; Aurrecoechea, Jose M.; Synthesis; vol. 45; 14; (2013); p. 2009 – 2017;,
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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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C6H3Cl2I

In a solution of 5.0 g of 3,5-dichloro-1-iodobenzene in 50 ml of t-butylmethylether, 12.2 ml of n-butyl lithium (1.58M hexane solution) was added dropwise at -78°C with stirring, after the completion of the addtion dropwise, stirred at the same temperature for 30 minutes. 6.6 g of chlorodifluoroacetic acid methyl ester was added dropwise at -78°C with stirring in the reaction mixture, after the completion of the addition drropwise, continued to stir at 0°C for further 30 minutes. After the completion of the reaction, the reaction mixture was poured in 100 ml of saturated ammonium chloride aqueous solution, extracted with ethyl acetate (100 ml x 1). The organic phase was dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure to obtain 4.6 g of crude aimed product as pale yellow oily substance. The resulting product was used as such without purification for the next step. 1H NMR (CDCl3, Me4Si, 300MHz) delta7.97 (s, 2H), 7.68 (s, 1 H).

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nissan Chemical Industries, Ltd.; EP1731512; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 40400-15-5, The chemical industry reduces the impact on the environment during synthesis 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, I believe this compound will play a more active role in future production and life.

isatin(1.0 mmol) was added to a 50 mL dry round bottom flask in turn.O-iodophenylacetonitrile (1.0 mmol), 4-hydroxycoumarin (1.0 mmol),Catalyst 3e (5 mol%), palladium dichloride (5 mol%),KOH (20 mol%), DMSO 3 mL, mix well, stir at 110 C,After the reaction was completed (TLC tracking), an appropriate amount of water was added and extracted with ethyl acetate.The organic phases are combined, and the excess solvent in the system is distilled off under reduced pressure.The crude product was separated by column chromatography (V petroleum ether: V ethyl acetate = 1:1 gradient elution) to give the title compound 12a in a yield of 88%

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-(2-Iodophenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangsu Normal University; Chen Wen; Yuan Rui; Cui Hao; Ren Xuanxuan; Zhou Shengliang; Wan Yu; Wu Hui; (19 pag.)CN109305970; (2019); A;,
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Electric Literature of 28547-29-7, 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. 28547-29-7, name is 2-Bromo-4-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 6 Preparation of ethyl 2-bromo-4-iodobenzoate (C60) To a stirred solution of 4-iodo-2-bromobenzoic acid (5.00 g, 15.3 mmol) in ethyl alcohol (100 mL) was added sulfuric acid (5 mL), and the reaction mixture was heated at 80 C. for 18 hours. The reaction mixture was cooled to 25 C. and concentrated under reduced pressure. The residue was diluted with ethyl acetate (2*100 mL) and washed with water (100 mL). The combined ethyl acetate extracts were washed with brine, dried over sodium sulfate, and concentrated under reduced pressure to afford the compound as a pale yellow solid (5.00 g, 92%): 1H NMR (400 MHz, DMSO-d6) delta 8.04 (d, J=1.2 Hz, 1H), 7.71 (d, J=7.6 Hz, 1H), 7.51 (d, J=8.4 Hz, 1H), 4.41 (q, J=7.2 Hz, 2H), 1.41 (t, J=7.2 Hz, 3H).

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-Bromo-4-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DOW AGROSCIENCES LLC; LePlae, JR., Paul Renee; Hunter, James E.; Watson, Gerald B.; Lo, William C.; Herbert, John; US2015/353477; (2015); A1;,
Iodide – Wikipedia,
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These common heterocyclic compound, 20776-54-9, name is 2-Amino-4-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. Product Details of 20776-54-9

Embodiment 22 2-amino-4-((4,4-dimethyl-1-oxothiochroman-6-yl)ethynyl)benzoic acid 1-oxo-6-ethynyl-4,4-dimethylbenzothiopyran (263mg, 1.0mmol) and 2-amino-4-iodobenzoic acid (262mg, 1.2mmol) were added to a flask, followed by addition of Pd(PPh3)2Cl2 (42mg, 0.06mmol) and CuI (23mg, 0.0412mmol). After the flask was purged with argon for 3 times to remove oxygen, 4mL dry DMF and 0.2mL dry Et3N were added via syringe. Then the reaction was continued at 70C for 8 h and monitored by TLC. After completion of the reaction, the reaction solution was cooled to room temperature and the reaction was quenched with saturated ammonium chloride solution. The mixture was diluted with ethyl acetate, washed with saturated ammonium chloride solution and saturated sodium chloride solution. The organic phase was dried over anhydrous sodium sulfate, filtered, concentrated and purified by flash column chromatography (PE:EtOAc = 50:1) to give the product (275 mg, 78%). 1H NMR (500 MHz, pyridine) delta 8.37 (d, J = 8.1 Hz, 1H), 7.92 (d, J = 8.0 Hz, 1H), 7.86 (s, 1H), 7.59 (s, 1H), 7.36 (s, 1H), 7.03 (d, J = 8.1 Hz, 1H), 5.67 (s, 1H), 3.20 – 3.14 (m, 1H), 3.11 – 3.05 (m, 1H), 2.38 (ddd, J = 14.2, 10.3, 1.7 Hz, 1H), 1.74 – 1.68 (m, 1H), 1.26 (s, 3H), 1.17 (s, 3H); 13C NMR (126 MHz, pyridine) delta 171.06, 152.34, 145.52, 140.46, 132.80, 131.65, 130.43, 130.20, 127.92, 126.32, 119.79, 118.58, 112.43, 91.82, 90.33, 55.01, 43.59, 34.63, 30.93, 30.63, 29.80. ESI(+)-MS: 354.3 [M+1]+.

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

Reference:
Patent; Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences; Huazhong University of Science and Technology; CAO, Xin; YU, Biao; WANG, Ning; CHEN, Junwei; (88 pag.)EP3428155; (2019); A1;,
Iodide – Wikipedia,
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