Category: iodides-buliding-blocks

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. 249647-24-3, name is Methyl 3-bromo-4-iodobenzoate, A new synthetic method of this compound is introduced below., Safety of Methyl 3-bromo-4-iodobenzoate

10.2. Methyl 2-bromo-2′,6′-dimethoxybiphenyl-4-carboxylate Stir a solution of 4.84 g (14,2 mmol) of methyl 3-bromo-4-iodobenzoate (J. Med. Chem., 1999, 42, 4088) and 3.88 g (21.29 mmol) of 2,6-dimethoxyphenyl boronic acid in 120 mL of DMF and 14.2 mL of a 2M aqueous solution of caesium carbonate for 15 minutes under argon, then add 984 mg (0.85 mmol) of Pd(PPh3)4 and heat for 2.5 h at 85 C. After concentration under reduced pressure, distribute the residue obtained in 600 mL of a 1:1 DCM/water mixture. Wash the organic phase with 100 mL of water, dry over MgSO4 and concentrate at reduced pressure. Purify the residue obtained by silica gel column chromatography, eluding with a heptane/EtOAc gradient from 0 to 10% of EtOAc. After concentration under reduced pressure, we obtain 2.79 g of methyl 2-bromo-240,6′-dimethoxybiphenyl-4-carboxylate in the form of oil. Yield=56%

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; Sanofi Aventis; US2009/318473; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 160976-02-3, 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 160976-02-3 as follows.

To a solution of 5-bromo-1,3-difluoro-2-iodobenzene (10.0 g, 0.048 mol) in N-methyl pyrrolidone (50 mL) was added CuCN (5.2 g, 0.057 mol). The reaction mixture was heated toreflux for 1.5 h. The reaction mixture was added EDTA, water and extracted with EtOAc. The organic layers were dried over Na2504 and concentrated to afford 1.6 g of title compound.

According to the analysis of related databases, 160976-02-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant Atmaram; MUTHUKAMAN, Nagarajan; PISAL, Dnyandeo; KHAIRATKAR-JOSHI, Neelima; SHAH, Daisy Manish; KADAM, Sheetal R; (303 pag.)WO2016/55947; (2016); A1;,
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. 6940-76-7, name is 1-Chloro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., Safety of 1-Chloro-3-iodopropane

Synthesis of compound 7c To a suspension of NaH (22 mg, 0.85 mmol) in DMF (2.0 mL) was added S1 (305 mg, 0.78 mmol)in DMF (1.5 mL). After 10 min at room temperature, S4a (0.20 mL, 1.53 mmol) was added to thismixture, and the reaction mixture was stirred at room temperature for 6 h, diluted with ether,washed with water and dried over Na2SO4. Purification by FCC (PE/EtOAc, 8 : 1) gave thechloride S5a (344 mg, 94%) as a yellow oil. 1H NMR (400 MHz, CDCl3) delta 7.81 (d, J = 1.8 Hz,1H), 7.80 (d, J = 7.9 Hz, 1H), 7.24 (dd, J = 1.8, 7.9 Hz, 1H), 3.74 (s, 6H), 3.54 (t, J = 6 Hz, 2H),3.23 (s, 2H), 1.98-1.94 (m, 2H), 1.80-1.73 (m, 2H); 13C NMR (100 MHz, CDCl3) delta 170.6, 151.7,143.4, 142.6, 130.6, 125.3, 86.3, 58.4, 52.7, 44.4, 37.9, 30.3, 27.6.

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 6940-76-7.

Reference:
Article; Gao, Yan; Shan, Dong; Jia, Yanxing; Tetrahedron; vol. 70; 34; (2014); p. 5136 – 5141;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 19099-54-8, 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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A DMF solution (8mL) of the o-substituted aryl iodide (0.36mmol), the o-bromobenzyl alcohol (0.36mmol) and norbornene (34mg, 0.36mmol) was added under nitrogen to a Schlenck-type flask, containing Pd(OAc)2 (4mg, 0.018mmol), the phosphine (0.036mmol), when required, and K2CO3 (124mg, 0.90mmol) or CsOPiv (211mg, 0.90). The reaction mixture was stirred at 105C for 24h. After cooling to room temperature the organic layer was diluted with EtOAc (20mL), washed twice with water (20mL) and dried over Na2SO4. The solvent was removed under reduced pressure and the resulting residue was purified by flash chromatography on silica gel using mixtures of hexane-EtOAc as eluent.

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-2-isopropylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Della Ca, Nicola; Fontana, Marco; Xu, Di; Cremaschi, Mirko; Lucentini, Riccardo; Zhou, Zhi-Ming; Catellani, Marta; Motti, Elena; Tetrahedron; vol. 71; 37; (2015); p. 6389 – 6401;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference 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

Some common heterocyclic compound, 791642-68-7, name is 4-Bromo-1-iodo-2-methoxybenzene, molecular formula is C7H6BrIO, 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. Formula: C7H6BrIO

To a solution of 4-bromo-1-iodo-2-methoxy-benzene (11.44 mmol, 3.581 g) in dryTHF (17.91 mL) under an atmosphere of nitrogen at -78C was added a solution ofisopropylmagnesium chloride in THF (1.3 mol/L, 11.0 mL, 14.30 mmol) over a period of 10 minutes, maintaining the reaction temperature between -65 and -70C. After stirring for 20 minutes, the reaction mixture was warmed to room temperature over one hour. The reaction mixture was cooled again to -78C and a solution of furan-2-carbaldehyde (13.73 mmol, 1.319 g) in THF (3.581 mL) was added over 5 minutes, whilst maintaining the reaction temperature between -65 and -70C. After 30 minutes, the reaction was allowed to warm to room temperature and stirred for a further 60 minutes. The reaction was quenched by the addition of saturated aqueous ammonium chloride. The aqueous layer was extracted with ethyl acetate, thecombined organic phase was dried over magnesium sulfate and the solvent removed in vacuo. The resulting residue was purified by silica gel flash chromatography (gradient elution: 0-30% ethyl acetate in hexane) to produce (4-bromo-2-methoxy- phenyl)-(2-furyl)methanol as an orange oil (1.55g, 48%). 1H NMR (400MHz, CDCI3) 7.42-7.34 (m, 1H), 7.26 (s, 1H), 7.17-7.09 (m, 1H), 7.06-6.98 (m, 1H), 6.39-6.28(m, 1H), 6.13-6.06 (m, 1H), 6.04-5.89 (m, 1H), 3.82 (s, 3H), 2.91 -2.60 (m, 1H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 791642-68-7, its application will become more common.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; HENNESSY, Alan, Joseph; HACHISU, Shuji; WILLETTS, Nigel, James; DALE, Suzanna, Jane; (70 pag.)WO2018/114584; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 19094-56-5, The chemical industry reduces the impact on the environment during synthesis 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, I believe this compound will play a more active role in future production and life.

In the l00mL hydrothermal synthesis reactor,Add sodium hydroxide (3 mmol), water (5 mL), stir and dissolve,Add 3-iodo-6-chlorobenzoic acid (0.5 mmol), cuprous oxide (0.05 mmol),White lignan (0.05 mmol), the reaction was stirred at 100 C for 6 hours.After cooling, the pH was adjusted to 2 with dilute hydrochloric acid and extracted with ethyl acetate.The extract is concentrated and subjected to column chromatography to obtain 2-chloro-5-hydroxybenzoic acid.71.6 mg, yield 83%.

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-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shenyang Pharmaceutical University; Yunnan Tropical Crop Science Institute; Chen Guoliang; Wu Ying; Bao Xuefei; Li Guohua; Liang Xinjie; Jiang Shikuan; Zhou Qifan; Du Fangyu; (11 pag.)CN109970542; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 76801-93-9, These common heterocyclic compound, 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, 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.

According to the compound of formula 1 and 3-chloro-1,2-propanediol,The molar ratio of sodium methoxide is 1:1:1.50 g of Compound Formula 1, 60 mL of methanol and 4.54 g of sodium methoxide were added to the reaction flask.3-chloro-1,2-propanediol 9.24g,Heat to 20-60 C for 10-20 hours.Distill off methanol and add 50 mL of water.Adjust the pH to 5-7 with hydrochloric acid,Add 80 mL of isopropanol and cool to 0-10 C.Precipitating crystals,dry,5-(2,3-Dihydroxypropyl)amino-N,N’-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-phthalamide solid (compound of formula 8),The purity is 95.6%.

The synthetic route of 76801-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Brethren Technology Co., Ltd.; Zhan Guowu; Xiong Anwei; Zhou Zhongping; Qian Zhida; (9 pag.)CN109912445; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 852569-38-1, These common heterocyclic compound, 852569-38-1, name is 5-Chloro-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.

Step 6.3. N-(5-chloro-4-fluoro-2-iodophenyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carboxamide Potassium t-butoxide (12.52 g, 111.6 mmol) is added at room temperature to a solution of 5-chloro-4-fluoro-2-iodoaniline (5.0 g, 22.3 mmol) in 250 mL of anhydrous THF under nitrogen. After stirring for 15 minutes, a solution of 1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carboxylic acid fluoride (5.67 g, 24.6 mmol) in 30 mL of anhydrous THF is added dropwise. The reaction mixture is stirred for 4 hours at room temperature and then poured into saturated aqueous NaHCO3 solution and extracted with EtOAc. The organic phase is washed with saturated aqueous NaCl solution, dried over Na2SO4 and concentrated to dryness. After purification by flash chromatography on silica (cyclohexene/EtOAc: 95/5 to 80/20), a red solid is obtained, which is purified by flash chromatography on amine phase (DCM) to give 2.84 g of a white solid (yield: 31%). LCMS (Method E): MH+= 404.0, RT = 2.29 min

Statistics shows that 5-Chloro-4-fluoro-2-iodoaniline is playing an increasingly important role. we look forward to future research findings about 852569-38-1.

Reference:
Patent; SANOFI; Benazet, Alexandre; Duclos, Olivier; Guillo, Nathalie; Lassalle, Gilbert; Macary, Karim; Viv, Valerie; EP2573073; (2013); A1;,
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. 612-55-5, name is 2-Iodonaphthalene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Iodonaphthalene

Bis(t?phenylphosphine)palladium (II) chloride (0 18 g, 0 26 mmol, 0 18 mol %) was added to a stirred solution of propargyl alcohol (8 43 mL, 144 8 mmol, 1 eq ), 2-iodonapthalene (36 g, 142 mmol), t?ethylamine (39 6 mL, 284 mmol, 2 eq ) and copper iodide (0 09 g, 0 49 mmol, 0 3 mol %) in tetrahydrofuran (750 ml) The mixture was stirred at 35 0C for 12 h under nitrogen atmosphere The mixture was then filtered through a bed of cehte and the filtrate was washed with ethyl acetate (200 ml) The filtrate was then concentrated in vacuo Purification by silica gel chromatography using 1 6 ethyl acetate/petrol as the eluting solvent afforded the desired compound (2 85 g, 1 1%) as a white solid 1H NMR (400 MHz, CDCl3) delta ppm 4 54 (2H, s, CH2), 7 45-7 49 (3eta, m, ArH), 7 75-7 81 (3eta, m, ArH), 7 95 (1eta, s, ArH)

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 612-55-5.

Reference:
Patent; DOV PHARMACEUTICAL, INC.; WO2008/57575; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com