Category: iodides-buliding-blocks

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. 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;,
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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;,
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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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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
Iodide – Wikipedia,
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Electric Literature of 627-31-6, The chemical industry reduces the impact on the environment during synthesis 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), I believe this compound will play a more active role in future production and life.

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 12 (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 chromtography (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, CDCI3) delta 7.26 (s, 1 H), 6.90 (s, 1 H), 6.68 (s, 1 H), 6.24 (d, 1 H, J = 15.3 Hz), 5.87 (d, 1 H, J = 8.9 Hz), 5.78 (m, 1 H), 5.53 (m, 1 H), 5.12 (m, 2H), 4.65 (m, 2H), 4.41 (m, 1 H), 4.1 1 (m, 1 H), 3.93 (s, 3H), 3.81 (m, 1 H), 3.40 (t, 2H, J = 6.7 Hz), 3.05 (dd, 1 H, J = 16.3, 10.1 Hz), 2.57 (m, 1 H), 2.34 (m, 2H), 1 .84 (d, 3H, J = 6.6 Hz), 0.92 (s, 9H), 0.28 (s, 3H), 0.26 (s, 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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SPIROGEN SARL; HOWARD, Philip Wilson; TIBERGHIEN, Arnaud; WO2013/53872; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 52548-14-8,Some common heterocyclic compound, 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, molecular formula is C8H7IO2, 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 1.1 kg of acetone to the 5L reaction flask.131g 2-iodo-5-methylbenzoic acid,Stir and dissolve,Add 350g of anhydrous potassium carbonate,After heating to reflux (55-60 C) for half an hour, add 114g 1,2,3-triazole,2.4 g of cuprous iodide.The reaction was kept under reflux (55-60 C) for 8 hours, sampled, and sampled once every 1 h. After the reaction was completed, it was cooled to room temperature for filtration, and the filter cake was washed twice with 120 g of acetone to obtain a white solid at room temperature (20-30 C). The white solid was dissolved in 1.3 kg of purified water and stirred.After 30 min, hydrochloric acid was added dropwise at room temperature to adjust the pH of the system to 1.5-2.0 to obtain a large amount of white solid. It was stirred for 1-2 hours, filtered, and the filter cake was washed twice with purified water. The resulting solid was dried to dryness at 50 ± 5 C to give a crude compound.Add 1 compound of crude product, 0.2 kg of absolute ethanol and 0 kg of purified water to a 1 L reaction flask, and warm to 75-80 C.Clear, heat for half an hour, cool to 0-5 C, filter, filter cake with a cold ethanol solution rinse, to obtain a white solid compound 1 boutique.The compound 1 was placed in a blast drying oven at a temperature of 55 C ± 5 C and dried for 5 h. Sampling, sampling every 2h 1Time, until the test (rapid moisture analyzer: 105 C, 10 min) loss on drying ? 0.5%, get Suwoleisheng intermediate products -Compound 1 was fine white crystalline solid 86 g, yield: 93%. Purity: 99.91%, Cu < 5 ppm. The synthetic route of 52548-14-8 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Yangzijiang Pharmaceutical Group Co., Ltd.; Zou Yiquan; Xu Jingren; Cai Wei; Xuan Jingan; Chen Lingwu; Ji Ye; Zhu Yunlong; Liu Jinfeng; Hu Tao; (8 pag.)CN109810067; (2019); A;,
Iodide – Wikipedia,
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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 35453-19-1 as follows. HPLC of Formula: C8H4I3NO4

5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1 ,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA to 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 500C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product. 13C NMR (DMSOcZ6) 66, 78.4, 148.9, 149.2, 169 MS (ES-) found 593.5 [M-H+], expected 593.7

According to the analysis of related databases, 35453-19-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GE HEALTHCARE AS; WO2007/133090; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 610-97-9,Some common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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.

To a stirred slurry of methyl 2-iodo-benzoate (5.0 g, 0.019 mol) and N-bromosuccinimide (3.74 g, 0.021 mol) in acetic acid (10 mL) was added concentrated H2SO4 (10 mL) dropwise, keeping the temperature at 20-40 C. The mixture was stirred at room temperature for 88 hours and then heated at 50 C. for 4 hours. The mixture was cooled to 10 C., treated with 40 g of ice water, and extracted with 50 mL of CH2Cl2. The organic phase was washed in succession with 2×50 mL 5% NaHCO3, 50 mL 10% Na2S2O3, 50 mL water, and concentrated to colorless oil. The residue was purified by column chromatography (silica gel, 10:90 EtOAc:hexane) to provide the title compound. 1H NMR (CDCl3, 400 MHz) delta 7.92 (d, J=4 Hz, 1H), 7.83 (d, J=8 Hz, 1H), 7.27 (dd, J=8, 4 Hz, 1H), 3.92 (s, 3H); MS (DCl/NH3) [M+NH4]+ at 358, [M+NH3.NH4]+ at 375.

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

Reference:
Patent; Altenbach, Robert J.; Black, Lawrence A.; Chang, Sou-jen; Cowart, Marlon D.; Faghih, Ramin; Gfesser, Gregory A.; Ku, Yi-yin; Liu, Huaqing; Lukin, Kirill A.; Nersesian, Diana L.; Pu, Yu-ming; Curtis, Michael P.; US2005/256309; (2005); A1;,
Iodide – Wikipedia,
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