Iodides-buliding-blocks

58755-70-7, name is 1-Iodo-4-methoxy-2-nitrobenzene, 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. name: 1-Iodo-4-methoxy-2-nitrobenzene

2-Iodo-5-methoxy-N-(4-methoxybenzyl)aniline (7f): 12 Iron (1.68 g, 30.0 mmol)was added in one portion to a stirred solution of NH4Cl (2.67 g, 500 mmol) in H2O(50 mL), and the resulting suspension was stirred at rt for 5 min. A solution of 1-iodo-4-methoxy-2-nitrobenzene (2.79 g, 10.0 mmol) in EtOH (100 mL) was then added, the resulting mixture was slowly warmed up to 60 C, and stirring was continued at this temperature for 2 h. The reaction mixture was filtered through a short pad of Celite, and the filtrate was extracted with EtOAc (3 × 50 mL). The combined organic fractions were washed with brine (100 mL), dried over anhydrous Na2SO4 and concentrated to give crude 2-iodo-5-methoxyaniline (2.35 g) as a brown oil, which was used in the next step without additional purification. From this material and 4-methoxybenzaldehyde (1.28 g, 9.44 mmol), compound 7f (2.89 g, 78% overtwo steps) was obtained according to GP1b as a colorless oil, which spontaneously crystallized when stored in a freeze

The synthetic route of 58755-70-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rassadin, Valentin A.; Scholz, Mirko; Klochkova, Anastasiia A.; De Meijere, Armin; Sokolov, Victor V.; Beilstein Journal of Organic Chemistry; vol. 13; (2017); p. 1932 – 1939;,
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Related Products of 25245-27-6,Some common heterocyclic compound, 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene, molecular formula is C8H9IO2, 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.

In a dry two necked flask were introduced N-[2-(1-Phenyl-cyclohexa-2,5-dienyl)-ethyl]-methanesulfonamide 3c (169 mg, 0.610 mmol), silver carbonate (336 mg, 1.22mmol), triphenylphosphine (24 mg, 0.092 mmol), 3,5-dimethoxy-iodobenzene 4b (322 mg, 1.22mmol), palladium acetate (6.8 mg, 0.030 mmol) and acetonitrile (24.5 mL). The mixture waswarmed to 85C and stirred for 16 hours. The mixture was filtered through celite, which wasthen washed with ethyl acetate. Evaporation of the solvents led to a paste, which was purifiedthrough silica gel chromatography (Petroleum ether/EtOAc 70:30), affording 5c as a white solid(98 mg, 39%). Mp = 123-125 C. IR (solid, KBr, numax, cm-1): 3295, 2936, 2255, 1606, 1454,1316, 1203, 1149, 1064, 973, 910, 777, 735, 710. 1H NMR (300 MHz, CDCl3): deltaH 1.53-1.63(1H, m, CHaHxCH2N), 1.90 (1H, d, 3JHH 6.0 Hz, CH cyclopropane), 1.93-2.00 (1H, m,CHaHxCH2N), 2.36 (1H, dta, JHH 6.0, 2.5 and 2.5 Hz, CH cyclopropane), 2.82 (3H, s,NSO2CH3), 3.00-3.10 (2H, m, CH2N), 3.19-3.23 (1H, m, CH cyclopropane), 3.78 (6H, s, OCH3 x2), 4.43 (1H, broad s, NH), 5.16 (1H, ddd, JHH 5.3, 2.2 and 1.5 Hz, CH olefinic), 5.91 (1H, dta, J= 5.3, 2.0 and 2.0 Hz, CH olefinic), 6.33 (1H, t, 4JHH 2.3 Hz, CH aromatic), 6.36 (1H, t, 4JHH 2.3Hz, CH x 2 aromatic), 7.17-7.35 (5H, m, 5CH aromatic). 13C NMR (75.5 MHz, CDCl3): 36.9(CH cyclopropane), 37.7 (C aliphatic), 37.9 (CH cyclopropane), 40.0 (NSO2CH3), (CH2N), 41.7(CH2CH2N), 51.3 (CH allylic), 55.4 (OCH3 x 2), 98.5 (CH aromatic), 105.8 (CH x 2 aromatic),126.6 (CH aromatic), 128.2 (CH x 2 aromatic), 131.6 (CH olefinic), 131.7 (CH x 2 aromatic),134.1 (CH olefinic), 137.5, 146.6 (2C aromatic), 160.9 (C x 2 aromatic). MS(SIMS) m/z (%):436 (M+Na, 35), 414 (M+H, 100), 305 (35). HRMS calcd for (M+H) C23H28NO4S 413.1661;found 413.1655 (1.5 ppm).

The synthetic route of 25245-27-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lebeuf, Raphael; Robert, Frederic; Landais, Yannick; ARKIVOC; vol. 2014; 3; (2013); p. 6 – 17;,
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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. 13421-13-1, name is 4-Chloro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 4-Chloro-2-iodobenzoic acid

General procedure: The solution of 2-iodobenzoic acid (2 mmol) in thionyl chloride (2 mL) was refluxed for 1h. After completion of the reaction, the liquid was removed under reduced pressure. Then the residue was dissolved with anhydrous DCM (1 mL) and added dropwise to the mixture (DCM (1 mL), triethylamine (6 mmol) and amine (2.4 mmol) or ammonium acetate (3 mmol)). After the reaction was completed by monitoring in TLC, water (20 mL) was added to the mixture and the aqueous phase was extracted with DCM (20 mL × 3). The combined organic layers were washed with HCl (aq.2 M), saturated NaHCO3 (aq.) and brine, dried with anhydrous Na2SO4, filtered and concentrated. The crude was washed (petroleum ether/dichloromethane = 50/1, v/v) and filtered to afford 1b-x.

The synthetic route of 13421-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Yingying; Zhou, Yang; Lei, Min; Hou, Jinjun; Jin, Qinghao; Guo, Dean; Wu, Wanying; Tetrahedron; vol. 75; 9; (2019); p. 1180 – 1185;,
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Application of 31599-61-8, These common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, 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: A mixture containing aryl halide (5.0 mmol), styrene(5.0 mmol), the palladium complex 5a (0.005 mmol) and potassium carbonate (1.06 g, 10.0 mmol) in methanol (20 ml) was refluxed for 2 h, as mentioned in Table 4. After the reaction, the solvent was evaporated, the product was poured into water, extracted with diethyl ether, dried over Na2SO4 and passed through a 1200 silica column (60-120 mesh). Upon evaporation of the ether, solid pure products were obtained. The yields of the products obtained from all the reactions were determined after isolation and the products characterized by 1H NMR spectra (Table 7).

Statistics shows that 4-Iodo-1,2-dimethylbenzene is playing an increasingly important role. we look forward to future research findings about 31599-61-8.

Reference:
Article; Pattanayak, Poulami; Pratihar, Jahar Lal; Patra, Debprasad; Brandao, Paula; Felix, Vitor; Chattopadhyay, Surajit; Polyhedron; vol. 79; (2014); p. 43 – 51;,
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Reference of 14452-30-3, 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. 14452-30-3, name is 1-(3-Iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In a 10 mL glass screw cap tube capped with a rubber septum, palladium acetate Pd(OAc)2, (5 mg, 0.023 mmol), 1,3-bis(diphenylphosphino)propane dppp, (9 mg, 0.023 mmol) were introduced under argon atmosphere. Then, 3 mL of freshly distilled toluene) were added under argon. The mixture was stirred for 10 min to allow formation of the catalyst. Then securinine 1 (100 mg, 0.46 mmol), potassium carbonate (K2CO3, 127 mg, 0.92 mmol) and the desired iodoarene (0.92 mmol) were added. The septum was replaced by a screw cap, and the mixture was stirred at 130 C, in an oil bath. After 24 h stirring, the reaction mixture was brought to room temperature and diluted with ethyl acetate (5 mL). The reaction mixture was filtered through a pad of Celite eluting with AcOEt (20 mL). The organic layer was extracted with a saturated aqueous solution of sodium hydrogen carbonate (10 mL) and brine (10 mL). The organic layer was then dried over anhydrous magnesium sulfate, filtered and concentrated to dryness. Purification by flash column chromatography on silica gel (pentane-ethyl acetate) affords the desired coupling product. 4.1.2.1.16 (6S,11aR,11bS)-5-(3-Acetylphenyl)-9,10,11,11a-tetrahydro-8H-6,11b-methanofuro[2,3-c]pyrido[1,2-a]azepin-2(6H)-one (2p) Yield: 60%. Orange oil; Rf 0.42 (petroleum ether-AcOEt, 50:50); [alpha]D20 – 475 (c = 0.10, CHCl3); 1H NMR (300 MHz, CDCl3): delta = 8.09 (s, 1H), 7.92 (d, J = 7.8 Hz, 1H), 7.69 (d, J = 7.8 Hz, 1H), 7.50 (dd, J = 7.8 Hz, 1H), 6.86 (d, J = 1.3 Hz, 1H), 5.59 (s, 1H), 4.36 (d, J = 4.3 Hz, 1H), 2.91-2.85 (m, 1H), 2.65-2.60 (m, 4H), 2.32-2.17 (m, 2H), 1.90-1.80 (m, 2H), 1.67-1.45 (m, 4H), 1.25-1.13 (m, 1H); 13C NMR (75 MHz, CDCl3): delta = 197.3, 173.6, 169.9, 149.2, 138.9, 137.5, 130.5, 129.2, 125.8, 116.3, 105.1, 89.0, 62.9, 61.6, 48.7, 41.8, 27.3, 26.5, 25.7, 24.0. MS (CI, NH3): m/z = 336 [M+ + H]; HRMS calcd for C21H21NO3H [M+ + H]: 336.15942; found: 336.15882, error = 1.8 ppm.

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-Iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Perez, Marc; Ayad, Tahar; Maillos, Philippe; Poughon, Valerie; Fahy, Jacques; Ratovelomanana-Vidal, Virginie; European Journal of Medicinal Chemistry; vol. 109; (2016); p. 287 – 293;,
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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. 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H4FIO2

General procedure: 1-acetoxyethanephosphonate-5-fluoro -1, 2- […] -3-(1H)-one (AFBX (2)) of synthetic The flask 2-iodo-5-fluorobenzoate 1330 mg (5mmol), then adding acetic acid 40 ml agitated until uniform. 3-hydroxybenzoic acid (purity 65%)overload Chloropyridin 1590 mg (6mmol) at a time and then adding a 24 60 C. The reaction liquid is cooled to 0 C, ether is added. The precipitate is filtered by deposition, vacuum drying in 1-acetoxyethanephosphonate-5-fluoro -1, 2- […] -3-(1H)-one (AFBX (2)) 770 mg (yield 48%)is obtained.

According to the analysis of related databases, 52548-63-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Tokyo Chemical Industry Co., Ltd.; Togo, Hideo; Inuma, Masataka; Moriyama, Katsuhiko; Takatsuki, Kenichi; (9 pag.)JP2015/63501; (2015); A;,
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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,
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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,
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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;,
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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;,
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