Category: iodides-buliding-blocks

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. 629-09-4, name is 1,6-Diiodohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 1,6-Diiodohexane

A suspension of sodium hydride (60%, 0.48 g, 12 mmol) in 20 ml of DMF was prepared. 1-(2-Chloro-5-thiazolylmethyl)-2-nitroiminoimidazolidine (2.61 g, 10 mmol) was added to this suspension. The resulting mixture was then stirred for 1 hour at room temperature. 1,6-Diiodohexane (1.64 g, 5 mmol) was added dropwise to this reaction mixture over the course of 30 minutes while cooling the reaction mixture with ice. Following completion of dropping, the mixture was stirred for 4 hours at room temperature. The DMF was distilled off from the reaction mixture under reduced pressure. The residue was then shaken with a mixture of water and chloroform. After separating the chloroform layer and drying, the solvent was distilled off under reduced pressure. The semi-solid residue was subjected to silica gel column chromatography with a mixture (15:1 (v/v)) of ethyl acetate and ethanol as the eluate. The crude product was recrystallized from methanol. The yield of crystalline product was 0.22 g (70%), and the melting point was 204 to 206 C. The results of elementary analysis and NMR analysis are shown below. [0117] Elementary Anal., Found (Calc.): C 36.80 (36.67), H 4.51 (4.33), N 23.50 (23.13). [0118] NMR (CDCl3, delta, ppm): 1.34 (4H, m), 1.60 (4H, m), 3.32 (4H, t, J=7.3), 3.66 (4H, m) , 3.77 (4H, m) , 4.57 (4H, s), 7.49 (2H, s). [0119] Based on the results of analysis, the compound of Example 14 was determined to be 1,6-bis[1-(2-chloro-5-thiazolylmethyl)-2-nitroiminoimidazolidin-3-yl]hexane having the structural formula indicated below.

The synthetic route of 629-09-4 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 1829-28-3, name is Ethyl 2-iodobenzoate, 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. Formula: C9H9IO2

In a test tube equipped with a stirring bar and a septum rubber,Under argon flow, bis (trifluoromethyl) zinc (DMPU) 2 complex (92 mg, 0.2 mmol),After adding copper (I) chloride (1.9 mg, 0.01 mmol), DMPU (0.2 ml) and ethyl 2-iodobenzoate (0.1 mmol, 16.6 mul)Replace septum rubber with screw cap,The reaction was carried out at 50 ° C. for 24 hours.After completion of the reaction,After cooling,As a result of quantification by 19 F-NMR using benzotrifluoride using the reaction solution as an internal standard substance,The yield of the objective ethyl 2- (trifluoromethyl) benzoate was 82percent.

The synthetic route of Ethyl 2-iodobenzoate has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 25309-64-2, name is 1-Ethyl-4-iodobenzene, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 25309-64-2, Recommanded Product: 1-Ethyl-4-iodobenzene

Step-1: Synthesis of tert-butyl (Z)-(2-(4-(2-(4-ethylphenyl)-l-(4-hydroxyphenyl)but-l-en-l- yl)phenoxy )ethyl)carbamate To a stirred solution of tert-butyl (E)-(2-(4-(l-(4-hydroxyphenyl)-2-(4,4,5,5-tetramethyl- l ,3,2-dioxaborolan-2-yl)but-l-en-l-yl)phenoxy)ethyl)carbamate (1.3 g, 2.55 mmol, Example- 46, Step-1) in 2-methyl THF (15 mL), l-iodo-4-ethylbenzene (0.651 mg, 2.8 mmol), 4M aqueous KOH (2 mL) and Pd(PPh3)2Cl2 (89 mg, 0.127 mmol) were added and the mixture was degassed with nitrogen for 15 min and heated at 85 C for 3 h. Upon completion, the reaction mixture was diluted with EtOAc. The organic layer was washed with water followed by brine, dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by silica gel chromatography (2:8 EtOAc in n- hexane) to give title compound (0.5 g, 40%).

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-Ethyl-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Electric Literature of 19099-54-8, These common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, 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.

0.3 mmol of sodium carbonate, 0.1 mmol of 1,2-bis(4-methoxyphenyl)acetylene, 0.005 mmol of palladium acetate, 0.005 mmol of bis(2-diphenylphosphinophenyl)ether, and pinacol borate 0.15mmol, 0.15mmol of 2-isopropyliodobenzene and 1mL of N,N-dimethylformamide were added to a 15mL reaction tube, and the nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C for 24 hours; cooling The reaction solution was diluted with ethyl acetate to room temperature.Wash three times with water, dry the organic phase with anhydrous Na2SO4, and filter.concentrate,Purification by thin layer chromatography gave 24.7 mg of the desired product.The yield was 51%. The nuclear magnetic and high resolution mass spectra of this compound are characterized as follows:

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

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (10 pag.)CN109879899; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 6940-76-7, A common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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.

To a solution of 2-fluoro-4-iodo-pyridine (7.70 g, 34.53 mmol, 1.00 eq) in tetrahydrofuran (80 mL) was added lithium diisopropylamide (2 M, 20.72 mL, 1.20 eq) at -78 C for 1.5 h. Then the mixture was added a solution of 1-chloro-3-iodo-propane (14.12 g, 69.06 mmol, 7.43 mL, 2.00 eq) in tetrahydrofuran (10 mL) at -78C and stirred for 0.5 h. Then the mixture was warmed to 15 C and stirred for 1 h. The mixture was quenched with saturated ammonium chloride solution (80 mL) and extracted with ethyl acetate (2 x 40 mL). The combined organic layers were washed with brine (50 mL), dried over sodium sulfate and concentrated to give a residue. The residue was purified by column chromatography (petroleum ether: ethyl acetate = 1:0 to 10:1) to give 3-(3-chloropropyl)-2-fluoro-4-iodo-pyridine (9.00 g, 30.05 mmol, 87% yield) as a light yellow oil.1H-NMR (400MHz, CDCl3) d 7.69 (d, J=5.6 Hz, 1H), 7.61 (d, J=5.2 Hz, 1H), 3.61 (t, J=6.4 Hz, 2H), 2.90 – 2.97 (m, 2H), 2.04 – 2.08 (m, 1H), 1.99 – 2.03 (m, 1H).

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; ARVINAS OPERATIONS, INC.; YALE UNIVERSITY; CREW, Andrew P.; HORNBERGER, Keith R.; WANG, Jing; CREWS, Craig M.; JAIME-FIGUEROA, Saul; DONG, Hanqing; QIAN, Yimin; ZIMMERMAN, Kurt; (1451 pag.)WO2020/51564; (2020); 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. 6213-88-3, name is (E)-Methyl 3-iodoacrylate, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 6213-88-3

Bis (benzonitrile) palladium(II) chloride (0.238 g, 0.62 mmol), t-butyl acetylene (1.31 g, 15.94 mmol) and copper (I) iodide (0.234 g, 1.26 mmol) were added at ambient temperature to a stirred solution of (E)-3-iodo- acrylic acid methyl ester (2.60 g, 12.26 mmol) in triethylamine (40 mL). The mixture was stirred at ambient temperature for 20 hours, diluted with saturated ammonium chloride solution and extracted with ethyl acetate. The combined organic layers were filtered through a short pad of celite, and the filtrate was dried over sodium sulfate and concentrated under reduced pressure. The crude material was purified by column chromatography to give the title compound as a light yellow oil (1.73 g, 85%). 1H-NMR (CDCl3.) delta: 1.26 (s, 9H), 3.74 (s, 3H), 6.13 (d, IH, J = 15.9Hz), 6.76 (d, IH, J = 15.9Hz).

According to the analysis of related databases, 6213-88-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AUSPEX PHARMACEUTICALS, INC.; WO2008/73863; (2008); A2;,
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. 135050-44-1, name is 3-Chloro-4-iodoaniline, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3-Chloro-4-iodoaniline

Diethyl 2-((3-chloro-4-iodophenylamino)methylene)malonate 3-Chloro-4-iodoaniline (3.0 g, 11.8 mmol) and diethyl 2- (ethoxymethylene)malonate (12.78 g, 59.2 mmol) were mixed in a 100 mL single neck flask, and the resulting mixture was heated to 120oC and stirred for 2.5 h. The mixture was allowed to cool to RT and purified by flash column chromatography on silica gel (10-20% ethyl acetate / petroleum ether) to afford the desired product (3.93 g) as a white solid. ESI-MS m/z : 422.1 [M – H]-.

According to the analysis of related databases, 135050-44-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ARAXES PHARMA LLC; LI, Liansheng; FENG, Jun; WU, Tao; REN, Pingda; LIU, Yi; LIU, Yuan; LONG, Yun, Oliver; WO2015/54572; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 2468-56-6, name is 6-Iodohex-1-yne, 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. COA of Formula: C6H9I

General procedure: A mixture of the corresponding precursor (1 eq) and alkylating agent (1.5 eq) and K2CO3 (2.5 eq) in DMF was stirred at rt till completion of the reaction. H2O was added and the mixture was extracted with EtOAc. The organic layer was dried, filtered and evaporated. The crude compound was used in next reaction step without further purification (it can be impure with the corresponding precursor).

The synthetic route of 6-Iodohex-1-yne has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Fundacion del Sector Publico Estatal Centro Nacional de Investigaciones Oncologicas Carlos III (F.S.P. CNIO); PASTOR FERNANDEZ, Joaquin Angel; BLASCO MARHUENDA, Maria Antonia; MARTINEZ GONZALEZ, Sonia; BLANCO-APARICIO, Carmen; GARCIA GARCIA, Ana Belen; VARELA BUSTO, Carmen; GOMEZ-CASERO ESTEBAN, Elena; BEJARANO BOSQUE, Leire; MENDEZ PERTUZ, Marinela; MARTINEZ RODRIGUEZ, Paula; GARCIA-BECCARIA, Maria; (71 pag.)EP3623370; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 33348-34-4, A common heterocyclic compound, 33348-34-4, name is 4-Amino-3-iodobenzonitrile, molecular formula is C7H5IN2, 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 an oven-dried three-necked round bottom flask provided with a reflux condenser was 4-Amino-3-benzonitrile (1.0 g, 4.1 mmol) dissolved in anhydrous THF (10 ml) under N2. BH3-THF was added dropwise. Once the addition was complete the reaction mixture was refluxed for 2h. The mixture was allowed to cool and HCl (2.0 N aq.) (6.0 ml) was added dropwise. Then the mixture was refluxed for 1.0 h. The solvents were removed under vacuum and residue was suspended in CH2Cl2 (30 ml). DMAP (100.1 mg, 0.8 mmol), Et3N (1.3 ml, 9.4 mmol) and BoC2O (2.7 g, 12.3 mmol) were added and the mixture stirred at r.t. for 1.5 h. H2O was added and the product extracted with EtOAc. The combined organic extracts were dried (MgSO4), filtered and concentrated. The crude product was purified by flash chromatography (CH2Cl2ZMeOH 99:1) affording 1.0 g (71%) of the title compound. 1H NMR (CDCl3) delta 7.55 (d, IH), 7.07 (dd, IH), 6.70 (d, 1 H), 4.76 (bs, IH),4.15 (d, 2H), 4.08 (bs, 2H), 1.46 (s, 9H).

The synthetic route of 33348-34-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RESPIRATORIUS AB; JOHANSSON, Martin; THORNQVIST-OLTNER, Viveca; TOFTERED, Joergen; WENSBO, David; DALENCE, Maria; WO2010/97410; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4387-36-4,Some common heterocyclic compound, 4387-36-4, name is 2-Iodobenzonitrile, molecular formula is C7H4IN, 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.

S1: The reaction formula of this step is as follows. The specific reaction operation is: at room temperature,Adding 100 mmol of the compound of the above formula (III) to an appropriate amount of the organic solvent N,N-dimethylacetamide (DMA),200 mmol of the compound of the above formula (IV), 0.4 mmol of palladium acetate,150 mmol of tetra-n-butylammonium bromide and 150 mmol of sodium carbonate,Then, the temperature was stirred to 120 ¡ã C, and the reaction was stirred at this temperature for 15 hours;After the reaction was completed, the reaction mixture was poured into a sufficient amount of ethyl acetate and then washed with saturated brine.The organic layer and the aqueous layer were separated, and the aqueous layer was sufficiently extracted with ethyl acetate.The organic layers are combined (ie, the organic layer washed with saturated brine and the organic layer obtained by ethyl acetate extraction).Dry with anhydrous Na2SO4 and distill under reduced pressure.The residue was eluted by flash column chromatography (a mixture of petroleum ether and ethyl acetate in a volume ratio of 8:1).The eluent was collected and evaporated to remove the eluent.The compound of the above formula (II) was obtained as a white solid in a yield of 87.8percent

The synthetic route of 4387-36-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou Medical University Affiliated The Second Hospital ? Wenzhou Medical University Affiliated Yuying Child Hospital; Wenzhou Medical University; Wang Zhiyi; Weng Jie; Chen Chan; Wang Zhibin; Zhou Zhiliang; Ma Jianshe; Xu Tong; (18 pag.)CN108250162; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com