Category: iodides-buliding-blocks

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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H3BrINO2

(1) Take 21.2g (100mmol) of 1-dibenzothiophene boronic acid,32.6g (100mmol) of 2-iodo-5-bromonitrobenzene,(1%) Pd (PPh3) 4,40g (300mmol) sodium carbonate,Toluene (800mL),Ethanol (200 mL) and water (200 mL),Heated to reflux, reacted for 8h, the reaction was completed;The reaction solution was extracted with ethyl acetate, and the organic phase was concentrated.A yellow solid A was obtained;

According to the analysis of related databases, 112671-42-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (28 pag.)CN110698458; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 181765-86-6 as follows. SDS of cas: 181765-86-6

phenanthrene-9-boronic acid (2.22 g, 10 mmol), methyl 5-bromo-2-iodobenzoate (3.41 g, 10 mmol), Pd (PPh3) 4 (0 · 21 g, 0 · 18 mmol), K2C03 solution were added to the reactor. (2 · 76g, 20mmol), deionized water 5mL, toluene 13mL, tetrahydrofuran 130mL, stirred and refluxed for 12h, after the reaction was terminated, the organic layer was separated, distilled under reduced pressure, purified by silica gel column and dried to give intermediate 7-1 ( 2.86g, 73%)

According to the analysis of related databases, 181765-86-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Dong Xiuqin; Cai Hui; (19 pag.)CN108774178; (2018); A;,
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. 58313-23-8, name is Ethyl-3-iodobenzoate, A new synthetic method of this compound is introduced below., Recommanded Product: Ethyl-3-iodobenzoate

To a solution of {l-{[(l,l-dimethylethyl)oxy]carbonyl}-5-[(phenylmethyl)oxy]-lH- indol-2-yl}boronic acid (1.13 g, 3.08 mmol), ethyl-3-iodobenzoate (0.34 mL, 2 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.126 g, 0.11 mmol), in 1,2- dimethoxyethane (35 mL) was added sodium carbonate (2 M) (4 mL, 8 mmol). The stirred reaction mixture was heated at reflux for 4 h under a nitrogen atmosphere. The reaction mixture was allowed to cool at room temperature and partitioned between water and ethyl acetate. The organic phase was separated, dried over magnesium sulfate, filtered, and the filtrate was concentrated to give an oil. The crude product was purified by flash chromatography over silica with a hexanes: ethyl acetate gradient (100:0 to 70:30) to give an oil. The oil was dissolved in dichloromethane and the solution was concentrated to give the product. The product was dissolved in ethyl acetate and one-half of the solution was concentrated to give 0.42 g of 1,1- dimethylethyl 2- {3-[(ethyloxy)carbonyl]phenyl} -5-[(phenylmethyl)oxy]- lH-indole- 1 – carboxylate for a total yield of 0.84 g (89%). 1U NMR (400 MHz, DMSO-J6): delta 7.99 (d, J = 9 Hz, IH), 7.95 (m, 2H), 7.75 (d, J = 8 Hz, IH), 7.58 (t, J = 8 Hz, IH), 7.45 (m, 2H), 7.37 (m, 2H), 7.31 (m, IH), 7.21 (d, J = 3 Hz, IH), 7.03 (dd, J = 9, 3 Hz, IH), 6.72 (s, IH), 5.13 (s, 2H), 4.32 (q, J = 7 Hz, 2H), 1.30 (t, J = 7 Hz, 3H), 1.23 (s, 9H). ES-LCMS m/z 494 (M + Na)+.

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; SMITHKLINE BEECHAM CORPORATION; WO2009/5998; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 628-77-3 as follows. Application In Synthesis of 1,5-Diiodopentane

Potassium carbonate (2.5 eq) was added to a solution of 8 (1.0 g, 1.72 mmol, 2.1 eq) and either 1,3-dibromopropane; 1,5-diiodopentane; or 1,3-bis(bromomethyl)benzene (1.0 eq) in DMF (5 mL). The resulting mixture was stirred at 75C for 3 days. After diluting with dichloromethane (25 mL), the inorganics were removed by filtration and the filtrate evaporated to dryness under reduced pressure. The residue was purified by flash chromatography to leave the products as white solids. i) diallyl 8,8′-(propane-1,3-diylbis(oxy))(2S,2’S, 11S, 11aS, 11’S, 11 a’S)-bis(2-(benzoyloxy)- 11-((tert-butyldimethylsilyl)oxy)-7-methoxy-5-oxo-2,3, 11, 11 a-tetrahydro-1H- benzo[e]pyrrolo[1,2-a][1,4]diazepine-10(5H)-carboxylate) 9a (gradient: ethyl acetate / heptane, 50/50 to 100/0 v/v). Yield 0.88 g (90%). LC/MS rt 2.17 min m/z (1227.4) M+Na.

According to the analysis of related databases, 628-77-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MEDIMMUNE LIMITED; HOWARD, Philip Wilson; HUTCHINSON, Ian; (102 pag.)WO2020/79239; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 108078-14-4, These common heterocyclic compound, 108078-14-4, name is 2-Iodo-3-methylbenzoic 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.

Example 289; 292 2912-iodo-3-methylbenzoic acid ethyl ester (289)A solution of the 2-iodo-3-methylbenzoic acid (6g-0.023mol) in EtOH (15OmL) is treated with concentrated HCl (2OmL) and refluxed for 48h. After removal of the EtOH in vacuo, the residue is diluted with water (125mL) and cooled to 00C in an ice bath. The pH is adjusted to 10 with solid NaOH pellets and extracted with EtOAc (3 x 75mL). The organic extracts are washed with water (2 x 5OmL) and brine (2 x 5OmL) and dried over MgSO4. Concentrated in vacuo to give the product as a pale yellow oil. (6g, 90%).LC/MS(ES+) m/z 291

Statistics shows that 2-Iodo-3-methylbenzoic acid is playing an increasingly important role. we look forward to future research findings about 108078-14-4.

Reference:
Patent; SANOFI-AVENTIS; WO2008/151211; (2008); 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.

Step A: H2S04 95-98% (2.54 ml_, 0.048 mol) was added to a solution of 2-iodo-5- methylbenzoic acid (25.0 g, 0.095 mol) in MeOH (220 ml.) and refluxed for 20h. The rxn mixture was cooled with an ice bath, and 1 N aq. NaOH was added dropwise until pH 8 was reached. The org. solvent was removed in vacuo and the aq. layer was extracted with DCM (2x). The combined org. extracts were washed with sat. aq. NaHC03 (1 x) and H20 (1x), dried (Na2S04), filtered and concentrated in vacuo to give methyl 2-iodo-5-methylbenzoate as a pale yellow liquid which was used in the next step without further purification. LC-MS A: tR = 0.87 min; [M+H]+ = 259.22.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-5-methylbenzoic acid, its application will become more common.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; BOLLI, Martin; BOSS, Christoph; BROTSCHI, Christine; GUDE, Markus; HEIDMANN, Bibia; SIFFERLEN, Thierry; WILLIAMS, Jodi T.; WO2014/57435; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-62-0, A common heterocyclic compound, 626-62-0, name is Iodocyclohexane, molecular formula is C6H11I, 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.

In the glove box, t-BuOLi (1 mmol, 2 equivalents, 80.1 mg) was added to the vial containing the stirrer in turn.B2pin2 (2mmol, 4 equivalents, 507.9mg), 0.85mL solvent methanol, 10muL H2O,Iodocyclohexane (0.5 mmol).The capped vial was removed from the glove box and the reaction mixture was stirred at 50 C for 48 hours. After cooling to room temperature, the reaction mixture was transferred to a test tube by methanol, and a certain amount of internal standard n-decane was added and diluted with ethyl acetate.The yield of the product cyclohexylboronic acid pinacol ester was determined by a GC-fid method to be 30%.

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; Peking University; Mo Fanyang; Sun Beiqi; Liu Qianyi; Hong Junting; (10 pag.)CN109575063; (2019); A;,
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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 19099-54-8

General procedure: Catalyst 1 (prepared according Ref.15a, 7.1 mg,0.05 mequiv of Pd) was added to a solution of aryl iodide (4 mmol,1.0 equiv), methyl acrylate (0.72 mL, 8 mmol, 2.0 equiv), Et3N (0.67 mL,4.8 mmol, 1.2 equiv) in a mixture of toluene (6.7 mL), DMF (3.3 mL) and H2O(0.1 mL). The reaction mixture was heated at 100 C for 20 h. After coolingto rt, 1 was filtered off under vacuum. The mixture of solvents wasconcentrated under vacuum and the residue was purified by flashchromatographyon silica gel to afford pure alkenes after drying under,vacuum (0.1 mbar).

The synthetic route of 19099-54-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Derible, Antoine; Becht, Jean-Michel; Le Drian, Claude; Tetrahedron Letters; vol. 54; 32; (2013); p. 4207 – 4209;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 98-61-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 98-61-3 name is 4-Iodobenzenesulfonyl chloride, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 16A; N-(3-{[(4-Iodophenyl)sulfonyl]amino}phenyl)acetamide; 4-Iodobenzylsulfonyl chloride (10.0 g) is provided in isopropanol (100 ml), sodium acetate (3.12 g), which is dissolved in a little water, is added and the mixture is stirred at room temperature for 30 min. N-(3-Aminophenyl)acetamide (4.96 g) is then added and the mixture is further stirred over night. The batch is diluted with water and a saturated sodium chloride solution and extracted with ethyl acetate. The organic phase is dried over sodium sulfate, concentrated and flash-chromatographed (eluent methylene chloride/methanol 1:0, 100:1, 80:1). 9.62 g (70% of theory) of product are obtained.HPLC (Method 6): Rt=4.14 minMS (ES+, ES-): m/z=417 [M+H]+, 415 [M-H]-,1H-NMR (400 MHz, DMSO-d6): delta=10.31 (s, 1H, NH), 9.91 (s, 1H, NH), 7.93 (d, 2H), 7.51 (d, 2H), 7.45 (s, 1H), 7.26 (d, 1H), 7.12 (t, 1H), 6.73 (d, 1H), 2.00 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Iodobenzenesulfonyl chloride, and friends who are interested can also refer to it.

Reference:
Patent; Svenstrup, Niels; Zimmermann, Holger; Karthaus, Dagmar; Goeller, Andreas; Heimbach, Dirk; Henninger, Kerstin; Lang, Dieter; Paulsen, Daniela; Riedl, Bernd; Schohe-Loop, Rudolf; Schuhmacher, Joachim; Wunberg, Tobias; US2009/176842; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 82777-09-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 82777-09-1 name is 2′-Iodo-1,1′:3′,1”-terphenyl, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

(2) Synthesis of Exemplified Compound A06 [0101] [Chem.[0102] The following reagents and solvents were charged into a 100-mL recovery flask. 21 -Iodo-m-terphenyl : 925 mg (2.60 mmol) TRP-Bpin2: 453 mg (0.943 mmol) Tetrakis (triphenylphosphine) palladium ( 0 ) : 80 mg (69 mu?iotaomicron) Toluene: 20 mLEthanol: 10 mL 30-wt% cesium carbonate aqueous solution: 10 mL This reaction solution was heat-refluxed for 3.5 hours while being stirred in a nitrogen atmosphere. After the reaction was completed, the reaction solution was added with water and was stirred, and a precipitated crystal was then filtrated, followed by performing washing with water, ethanol, and acetone, so that a crude product was obtained. Next, after this crude product was heated and dissolved in toluene, this solution thus obtained was filtrated while being hot, and recrystallization was then performed using toluene as a solvent. After the crystal thus obtained was vacuum dried at 150 C, sublimation refining was performed at a pressure of 10~4 Pa and a temperature of 360C, so that 251 mg of a high-purity exemplified compound A06 was obtained (yield: 39%) . [0103] The result of identification of the obtainedcompound is shown below. [MALDI-TOF-MS] Observed value: m/z=684.35, Calculated value:[1H-NMR (400 MHz, CDC13) ]delta 8.07 (d, 2H) , 8.04 (d, 2H) , 7.99 (dd, 2H) , 7.57-7.45 (m, 6H) , 7.41 (dd, 2H) , 7.18-7.00 (m, 22H) . In addition, the Tl energy (equivalent wavelength) of the exemplified compound A06 was 469 nm measured by a method similar to that of Example 1. [0104] When the energy gap of the exemplified compound A06 was further measured by a method similar to that of Example 1, the absorption edge of the absorption spectrum was 363 nm, and the energy gap of the exemplified compound A06 was 3.42 eV. [0105] When the ionization potential of the exemplified compound A06 was further measured by a method similar to that of Example 1, the ionization potential of theexemplified compound AO 6 was 6.34 eV. [0106] Furthermore, when the LUMO level of the exemplified compound A06 was estimated by a method similar to that of Example 1, it was estimated to be -2.92 eV.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2′-Iodo-1,1′:3′,1”-terphenyl, and friends who are interested can also refer to it.

Reference:
Patent; CANON KABUSHIKI KAISHA; KOSUGE, Tetsuya; KAMATANI, Jun; KISHINO, Kengo; TOMONO, Hiroyuki; WO2011/132624; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com