Continuously updated synthesis method about C2H2IN

The chemical industry reduces the impact on the environment during synthesis 2-Iodoacetonitrile. I believe this compound will play a more active role in future production and life.

Electric Literature of 624-75-9, 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. 624-75-9, name is 2-Iodoacetonitrile, This compound has unique chemical properties. The synthetic route is as follows.

To a mixture of 5-bromo-2-isopropyl-4-methoxy- phenol from step 4(0.831 g, 34 mmol) and K2C03 (0.562 g, 4.1 mmol) in 17 mE dimethyl formamide (DMF) was added iodoacetonitrile (0.594 g, 3.6 mmol). The mixture was warmed to 60 C. for 30 minutes and then allowed to cool to room temperature. After cooling to room temperature the mixture was taken up in SOmE of H20 and extracted with 1:1 toluene/ethyl acetate, washed with H20 and then with brine. The combined organic layers were dried over Na2504, filtered and concentrated in vacuo to give a crude solid. Purification via flash chromatography (1:1 hexane/CH2C12) afforded (5-bromo-2-isopropyl-4-methoxy-phenoxy)-aceto- nitrile (0.611 g, 63%) as a while solid.

The chemical industry reduces the impact on the environment during synthesis 2-Iodoacetonitrile. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Ford, Anthony P.; McCarthy, Bruce G.; US2015/57299; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Sources of common compounds: 1,4-Diiodobutane

The synthetic route of 1,4-Diiodobutane has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 628-21-7, name is 1,4-Diiodobutane, 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. Safety of 1,4-Diiodobutane

Step (a): Synthesis of 1-(4-amino-phenyl)cyclopentanecarboxylic acid methyl esterSodium hydride (2.8 g, 60% dispersion in mineral oil) was added slowly to an ice-cold solution of (4-nitro-phenyl)-acetic acid methyl ester (6.0 g, 30.7 mmol) in anhydrous DMF (30 mL) under nitrogen atmosphere. After stirring at 0 C. for 20 min, 1,4-diiodobutane (7.86 mL, 61 mmol) was added drop wise under stirring. After complete addition, the reaction mixture was warmed to about 20-35 C. and stirring continued for an additional 3 h. The reaction was stopped by adding water drop wise followed by EtOAc. The organic layer was separated, washed with brine, dried over sodium sulfate, and concentrated under reduced pressure. The material was purified by chromatography over silica gel to afford a pale yellow viscous liquid that solidified on standing at about 20-35 C. (4.1 g, 54% yield). The solid (3.4 g, 13.6 mmol) was dissolved in anhydrous ethanol and tin (II) chloride dihydrate (13.86 g, 61 mmol) was added slowly under nitrogen atmosphere. Thereafter, the mixture was heated at 90 C. for 3 h. After evaporation of volatiles under reduced pressure the resultant mixture was diluted with ice water, and the solution was adjusted to pH 11 by adding NaOH (aq). The mixture was extracted with EtOAc (3×50 mL) and the combined organic extracts were washed with water, brine, dried over sodium sulfate, and concentrated under reduced pressure to afford the title compound as a granular light yellow solid (2.67 g, 88% yield).1H NMR (CDCl3, 300 MHz): delta 7.16 (dd, J=8.4, 1.8 Hz, 2H), 6.63 (dd, J=8.4, 1.8 Hz, 2H), 3.59 (s, 3H), 2.60-2.55 (m, 2H), 1.87-1.67 (m, 6H).LC-MSD (ES+): m/z [220 (M+H)+, 100].

The synthetic route of 1,4-Diiodobutane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dr. Reddy’s Laboratories Ltd.; US2010/144722; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some scientific research about 101335-11-9

The synthetic route of 101335-11-9 has been constantly updated, and we look forward to future research findings.

101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, 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. Recommanded Product: 101335-11-9

The 1-(2-chloro-4-fluorophenyl)-2-piperazinone used in the above procedure was prepared as follows: A suspension of 2-piperazinone (1.5 g, 15.0 mmol), 2-chloro-4-fluoro-1-iodobenzene (3.8 g, 15.0 mmol), copper(l) iodide (0.57 g, 3.0 mmol), N,N’-dimethyl-1 ,2- cyclohexanediamine (1.3 g, 6.0 mmol), and potassium phosphate (6.4 g, 44.9 mmol) in 1 ,4-dioxane (20 ml) was heated at reflux (1000C) under argon for 20 hours. The mixture was allowed to cool to room temperature and then diluted with dichloromethane and 0.88M ammonia diluted in water (1 :5). The mixture was extracted into dichloromethane (x3), and then the combined organic extracts were washed with water (x2) and dried over magnesium sulphate. The solvent was evaporated in vacuo and the crude product was purified by flash-silica gel chromatography, eluting with 5% 2M ammonia in methanol in dichloromethane, to give the product 1-(2-chloro-4-fluorophenyl)-2-piperazinone (250mg) as a brown oil which was used without further purification. LC/MS [M+H]+ = 229.

The synthetic route of 101335-11-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/53459; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Introduction of a new synthetic route about 4949-69-3

The synthetic route of 4-Iodo-3-methylaniline has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 4949-69-3, name is 4-Iodo-3-methylaniline, 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. HPLC of Formula: C7H8IN

Example 7; N-(3-{8-(2.6-DifluorophenylV7-oxo-2-r(2,2,6.6-tetramethyl-4-piperidinyl’)aminol-5,6,7, 8-tetrahydropyrimido[4,5-(/1pyrimidin-4-yl|-4-methylphenyl)-3- thiophenecarboxamide; 7a) N-Q -iodo-4-methyrphenyl)-3 -thiophenecarboxamide; 3-Thiophenecarboxylic acid (2.O g, 15.6 mmol) was dissolved in methylene chloride (100 mL) and 2 drops of DMF were added. The mixture was cooled to 0 0C and oxalyl chloride (1.5 mL, 17.1 mmol) was added slowly and allowed to warm to room temperature. Gas evolution was observed during warming. 3-Methyl-4- iodoaniline (5.45 g, 23.5 mmol), 4 drops of pyridine and K2CO3 (2.58 g, 18.7 mmol) are dissolved in CH2Cl2 (10 mL) and cooled to about 00C. After about Ih, the acid chloride mixture is slowly added to the cooled aniline mixture and allowed to warm to room temperature and stirred for about 18h. The resulting mixture is filtered, washed with ethyl acetate and the filtrate is concentrated to a brown oil. The crude EPO material was purified via flash chromatography (10-30% ethyl acetate in hexanes) to afford the title compound (1.56 g, 29%) as an off-white solid.

The synthetic route of 4-Iodo-3-methylaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/104889; (2006); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

New learning discoveries about 103962-05-6

According to the analysis of related databases, 103962-05-6, the application of this compound in the production field has become more and more popular.

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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 103962-05-6

Example 1A 2-(4-(trifluoromethoxy)phenyl)malononitrile To a suspension of sodium hydride (2.87 g, 114 mmol) in THF (15 mL), malononitrile (4.77 mL, 76 mmol) in 2 mL of THF was added dropwise at 0 C. After the gas evolution ceased, 1-iodo-4-(trifluoromethoxy)benzene (5.92 mL, 37.8 mmol) and bis(triphenylphosphine)palladium(II) chloride (0.797 g, 1.135 mmol) were added. This mixture was then heated at reflux under nitrogen overnight. The suspension was cooled to ambient temperature, treated with water, acidified with 1N HCl and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate and filtered. The filtrate was concentrated and purified on silica gel (0-30% ethyl acetate in hexanes) to give 8.2 g of product as a tan solid. 1H NMR (400 MHz, CDCl3) delta ppm 7.48-7.65 (m, 2H) 7.37 (d, J=8.35 Hz, 2H) 5.09 (s, 1H). MS (ESI) m/z 225.1 (M-H)-.

According to the analysis of related databases, 103962-05-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ABBOTT LABORATORIES; US2012/122888; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Extended knowledge of 26670-89-3

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Related Products of 26670-89-3,Some common heterocyclic compound, 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, molecular formula is C7H6BrI, 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.

(2-2) Synthesis of 2-Bromo-1-Methyl-4-Phenylbenzene (0144) A mixture of 2-bromo-4-iodotoluene (14.5 g) obtained by the step (2-1), phenylboronic acid (6.35 g), tetrakis(triphenylphosphine)palladium (0) (1.69 g), potassium carbonate (20.2 g), 1,4-dioxane (117 mL), and water (13 mL) was refluxed for 3 hours in an argon atmosphere. The resulting reaction mixture was returned to room temperature, and extracted with dichloromethane. The organic layer was washed with a saturated sodium chloride solution, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 2-bromo-1-methyl-4-phenylbenzene (8.6 g). The yield was 71%.

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; ITO, Hirokatsu; KAWAMURA, Masahiro; MIZUKI, Yumiko; HAKETA, Tasuku; HAYAMA, Tomoharu; TAKAHASHI, Ryota; (141 pag.)US2017/183291; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Simple exploration of 35674-27-2

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Adding a certain compound to certain chemical reactions, such as: 35674-27-2, name is 4-Iodo-3-nitrobenzoic acid, 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 35674-27-2, Recommanded Product: 4-Iodo-3-nitrobenzoic acid

a. 4-iodo-3-nitro-benzophenone 5.3 g (17 mmol) of 4-iodo-3-nitrobenzoic acid and 8.0 g (60 mmol) of aluminium trichloride are added successively to 70 ml of benzene while cooling with an ice bath. Then the mixture is stirred for 2 hours at ambient temperature, then poured into ice water, extracted with methylene chloride, dried with sodium sulphate and concentrated in vacuo. Yield: 5.4 g (90% of theory), Rf value: 0.83 (silica gel; ethyl acetate/petroleum ether=3:7)

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Boehringer Ingelheim Pharma KG; US6479524; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 1643-29-4

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, 3-(4-Iodophenyl)propanoic acid, other downstream synthetic routes, hurry up and to see.

Application of 1643-29-4, 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. 1643-29-4, name is 3-(4-Iodophenyl)propanoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 3-(p-iodophenyl)propanoic acid (63 mg, 0.22 mmol) and EDC.HC1 (57 mg, 0.30 mmol) in CH2C12 (5 mE) was added NEt3 (84 pL, 0.60 mmol) and the reaction was stirred at it under Ar for 30 mm. Then a solution of EuO.3OtBu (2) (103 mg, 0.22 mmol) in CH2C12 (1 mE) was added and the reaction was stirred overnight at it under Ar. The reaction was diluted with 10 mE CH2C12 and washed successively with H20 and saturated NaC1 solution. The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure to give the crude product as a pale oil. The crude product was purified by flash chromatography (100% hexane to 100% EtOAc over 20 mm), and EuO-IPPA.3OtBu (6) was isolated as a clear oil (87 mg; 53%). ?H NMR (500 MHz, CDC13) oe 7.57 (d, 2H, J=8.2 Hz), 6.96 (d, 2H, J=8.2 Hz), 6.61 (br s, 1H), 5.61 (d, 1H, J=8.2 Hz), 5.44 (d, 1H, J=7.8 Hz), 4.34 (m, 1H), 4.23 (m, 1H), 3.29-3.16 (m, 2H), 2.90 (t, 2H, J=7.8 Hz), 2.46 (t, 2H, J=7.8 Hz), 2.27 (m, 2H), 2.09 (m, 1H), 1.85 (m, 1H),1.73 (m, 1H), 1.58-1.40 (m, 3H), 1.46 (s, 9H), 1.42 (s, 18H). ESI(+)=732.4 [M+H]. Calculated mass: 731.3

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, 3-(4-Iodophenyl)propanoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Cornell University; Babich, John W.; Kelly, James M.; Amor-Coarasa, Alejandro; Ponnala, Shashikanth; (36 pag.)US2017/368005; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Brief introduction of C8H6FIO

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 914225-70-0, its application will become more common.

Some common heterocyclic compound, 914225-70-0, name is 1-(5-Fluoro-2-iodophenyl)ethanone, molecular formula is C8H6FIO, 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: C8H6FIO

Step 1 : A solution of (-)-DIPCI ((-)-B-chlorodiisopinocampheylborane) (57.1 g, 178 mmol) in THF (tetrahydrofuran) (100 ml) was cooled to -20 to -30 C. A solution of compound 1 (31 .3 g, 1 19 mmol) in THF (100 ml) was then added dropwise, via addition funnel (30 min addition). The reaction was left to warm up to room temperature (RT). After 2 h, the reaction was cooled to -30 C and another portion of (-)-DIPCI (38.0 g, 1 19 mmol) was added. After 30 min, the reaction was allowed to warm to RT and after 1 h, the solvents were removed in vacuo and the residue re-dissolved in MTBE (methyl tertiary-butyl ether) (200 ml). A solution of diethanolamine (31 g, 296 mmol) in ethanol/THF (15 ml/30 ml) was added via addition funnel, to the reaction mixture under an ice bath. The formation of a white precipitate was observed. The suspension was heated at reflux for 2 hours then cooled to room temperature, filtered and the mother liquids concentrated in vacuo. The residue was suspended in heptane/EtOAc (7:3, 200 ml) and again filtered. This procedure was repeated until no more solids could be observed after the liquids were concentrated. The final yellow oil was purified by column chromatography (eluent: cyclohexane/EtOAc 99:1 to 96:4). The resulting colorless oil was further purified by recrystallization from heptanes, to give alcohol compound 2 (25 g, 80% yield, 99% purity and 96% ee) as white crystals. 1H NMR (400 MHz, CDCI3) delta 7.73 (dd, 1 H), 7.32 (dd, 1 H), 6.74 (ddd, 1 H), 4.99 – 5.04 (m, 1 H), 2.01 (d, 1 H), 1 .44 (d, 3 H). LCMS-ES: No ionization, Purity 99%. Chiral GC (column CP-Chirasil-DexnCB): 96% ee; Rt (minor) 17.7 minutes and Rt (major) 19.4 minutes.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 914225-70-0, its application will become more common.

Reference:
Patent; PFIZER INC.; JENSEN, Andrew, James; LUTHRA, Suman; RICHARDSON, Paul, Francis; WO2014/207606; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Discovery of 4-Bromo-1-iodo-2-nitrobenzene

The synthetic route of 112671-42-8 has been constantly updated, and we look forward to future research findings.

Related Products of 112671-42-8, These common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, 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.

Under anaerobic conditions, In 1 liter single-necked flask was charged with 100 g of compound 7, 2-thiophene boronic acid pinacol ester, 64g, Na2CO3 (20g, 184 mmol) in tetrahydrofuran (500 mL), and deionized water (50 mL), catalyst Pd (PPh3) 4 (5 g, 4.3 mmol). The mixture was stirred at 90 C for 3 days and night. The organic compound was added with 3 liters of deionized water and extracted three times with CH2Cl2 (3 X 1000 mL). The extract was dried with anhydrous Na2SO4 for four hours and the solvent was evaporated with a rotary evaporator. The residue was separated by 300 mesh analytical silica gel column and eluted with CH2Cl2 / n-hexane (1: 10). The effluent was evaporated to dryness to give the product 8 as a yellow oily liquid (63 g,)

The synthetic route of 112671-42-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Henan Normal University; Qin Ruiping; Jiang Yurong; Zhang Kaixuan; Zhang Haoxing; Zhang Qunying; (7 pag.)CN104098591; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com