Tag: M.W=200-300

Electric Literature of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A resealable tube was charged with 3-iodo-4-methylbenzoic acid (0.4 g 1.5 mmol) and thionyl chloride (4.0 ml, 46.2 mmol). The vessel was purged with argon and sealed. The mixture was heated at 80 C. for 1 hour. The reaction was cooled and then concentrated to a brown solid. The solid was dissolved in 6 ml of CH2Cl2, and added to a solution of the N-(3-amino-2-methylphenyl)-2-morpholinoacetamide (0.41 g, 1.6 mmol) in 4 ml of CH2Cl2. To this was then added triethylamine (0.62 ml, 0.46 g, 4.5 mmol). The reaction was stirred at room temperature for 16 hours. The resulting precipitate was filtered, washed with CH2Cl2 and dried under high vacuum to afford 3-iodo-4-methyl-N-(2-methyl-3-(2-morpholinoacetamido)phenyl)benzamide as a white solid. MS m/z=494.0 [M+H]+; Calc’d for C21H24IN3O3: 493.

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

Reference:
Patent; Amgen Inc.; US2007/54916; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, molecular formula is C7H6FI, 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. Recommanded Product: 39998-81-7

2-Fluoro-4-iodobenzoic acid (Compound B) A round bottom (RB) flask containing a solution of 8.0 g (27.0 mmol) of sodium dichromate in 44 mL of glacial acetic acid was placed in an external water bath (21 C.) and left exposed to air. To the resultant orange slurry was added 3.2 g (13.6 mmol) of 2-fluoro-4-iodotoluene followed by the dropwise addition of 22 mL of c. sulfuric acid via syringe (caution: if added too quickly there is a tendency for the mixture to erupt). After the addition of approximately 8 mL of sulfuric acid, a green solid precipitated and the water bath temperature had risen (25 C.). The green reaction mixture was heated in an oil bath (90 C.) for one hour, allowed to cool to ambient temperature, diluted with 1N NaOH solution (aq.) and ethyl acetate (500 mL) and then quenched with sat. NaHCO3 (aq.) solution. The organic phase was separated and washed with water and brine, dried over MgSO4, filtered and concentrated in vacuo to an orange oil. Residual acetic acid was removed by further extraction between ethyl acetate and sat. NaHCO3 (aq.) solution and washing of the organic phase with water and brine. The organic phase was dried over MgSO4, filtered and concentrated in vacuo to give the title compound as an orange solid. PMR (DMSO-d6): delta 7.61 (1H, t, J=8.0 Hz, J (C-F)=8.0 Hz), 7.67 (1H, dd, J=1.5, 8.2 Hz), 7.78 (1H, dd, J=1.5 Hz, J (C-F)=8.9 Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 39998-81-7, its application will become more common.

Reference:
Patent; Allergan Sales, Inc.; US6037488; (2000); 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. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., name: 1-Chloro-3-iodopropane

6-Fluoro-5-methyl-1-[3-(4-propoxypiperidin-1-yl)propyl]-3,4-dihydro-1H-quinolin-2-one (107LH95-2) A reaction flask was charged with 6-fluoro-5-methyl-3,4-dihydro-1H-quinolin-2-one (0.090 g, 0.50 mmol) in dry DMF (0.5 mL) under N2. NaH (60% in oil, 0.023 g, 0.55 mmol) was added and stirred at rt for 30 min. Then 3-chloro-1-iodopropane (0.079 g, 0.50 mmol) was added followed by stirring at r.t for 20 h. The reaction mixture was quenched with water and the product extracted into EtOAc. The combined organic layers were dried over Na2SO4, filtered, and concentrated. The crude material was dissolved in MeCN (2 mL) followed by addition of 4-propoxypiperidine (0.086 g, 0.6 mmol), NaI (0.150 g, 1.0 mmol), and K2CO3 (0.138 g, 1.0 mmol) and shaken at 50 C. for 20 h. The reaction mixture was quenched with water and the product extracted into EtOAc. The combined organic layers were dried over Na2SO4, filtered, and concentrated. The residue was purified by cation-exchange CC followed by flash CC (SiO2; EtOAc) to give the title compound (107LH95-2) (0.074 g, total yield 41%). 1H NMR (CH3OD) delta 7.03 (dd, J=4.8, 9.2 Hz, 1H), 6.99-6.92 (m, 1H), 3.98 (brt, J=7.4 Hz, 2H), 3.46-3.38 (m, 3H), 2.95-2.84 (m, 4H), 2.64-2.42 (m, 6H), 2.20 (d, J=2.0 Hz, 3H), 1.98-1.83 (m, 4H), 1.72-1.30 (m, 4H), 0.92 (t, J=7.4 Hz, 3H); 13C NMR (CH3OD) delta 171.1, 157.7 (d, J=240 Hz), 135.4 (d, J=3 Hz), 128.1 (d, J=4 Hz), 122.8 (d, J=18 Hz), 114.1, (d, J=9 Hz), 113.0 (d, J=25 Hz), 73.1, 69.7, 55.0, 50.3, 40.3, 30.8, 29.9, 23.9, 23.1, 22.7, 21.4, 9.8 (br).

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Skjaerbaek, Niels; Koch, Kristian Norup; Mikael Friberg, Bo Lennart; Tolf, Bo-Ragnar; US2005/209226; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

333447-42-0, name is 1,5-Difluoro-2-iodo-4-methylbenzene, 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. Quality Control of 1,5-Difluoro-2-iodo-4-methylbenzene

A solution of 1,5-difluoro-2-iodo-4-methylbenzene (26, 7.11 g, 28.0 mmol), Zn(CN)2 (1.97 g, 16.8 mmol) and Pd(PPh3)4 (3.23 g, 2.8 mmol) in DMF (40 mL) was heated at 90 C for 1.5 h. The reaction mixture was concentrated in vacuo and the residue was taken in water (400 mL) and extracted with ether (400 mL). The combined organic layer was washed with excess aq ammonium hydroxide solution. The separated organic layers were dried and purified b chromatography to yield purified product which contained triphenylphospine oxide. The crude mixture was further purified by sublimation (45 C, 1 mm/Hg) to yield 27 (1.8 g, 42%) as a colorless solid. 1H NMR (400 MHz, CDCl3) delta 7.47 (t, 1H, J = 8.0 Hz), 6.92 (t, 1H, J = 9.2 Hz), 2.27 (s, 3H).

The synthetic route of 333447-42-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Venkatraman, Srikanth; Velazquez, Francisco; Gavalas, Stephen; Wu, Wanli; Chen, Kevin X.; Nair, Anilkumar G.; Bennett, Frank; Huang, Yuhua; Pinto, Patrick; Jiang, Yueheng; Selyutin, Oleg; Vibulbhan, Bancha; Zeng, Qingbei; Lesburg, Charles; Duca, Jose; Heimark, Larry; Huang, Hsueh-Cheng; Agrawal, Sony; Jiang, Chuan-Kui; Ferrari, Eric; Li, Cheng; Kozlowski, Joseph; Rosenblum, Stuart; Shih, Neng-Yang; George Njoroge; Bioorganic and Medicinal Chemistry; vol. 22; 1; (2014); p. 447 – 458;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3930-83-4,Some common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, molecular formula is C7H6INO, 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.

At room temperature,A reaction tube equipped with a stirring magnet was charged with 0.2 mmol of the compound represented by the formula (I-2)0.005 mmol catalyst Dichloro (p-cymene) ruthenium dimer ([RuCl2 (cymene)] 2),0.24 mmol cesium acetate,Then purged with nitrogen,Under nitrogen protection was added 1mL isopropanol,Stirring heated to 100 ,And reacted at this temperature for 20h.After the reaction,The reaction solution was cooled to room temperature,Filtration with a layer of silica gel funnel,Then, the solvent was distilled off under reduced pressure,The residue was purified by flash column chromatography (petroleum ether / ethyl acetate,Both volume ratio of 1: 1) purification,Thus, the target dehalogenation product represented by formula (III-2) was obtained.Calculated,The yield is 98%.

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

Reference:
Patent; Wenzhou University; Xia Yuanzhi; You Tingjie; (11 pag.)CN106588687; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 90347-66-3, A common heterocyclic compound, 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, molecular formula is C9H9IO2, 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.

Methyl 3-iodo-4-methylbenzoate (SM1) (30 g, 0.471 mol) was dissolved in tetrahydrofuran (1200 mL). plusTrimethylsilylacetylene (92.3 g, 0.942 mol) and diisopropylethylamine (72.9 g, 0.565 mol) were added. System vacuum,Then fill with nitrogen. Cuprous iodide (8.92 g, 0.047 mol) and bistriphenylphosphinepalladium dichloride (16.5 g, 0.024 mol) were added.The system is evacuated and filled with nitrogen. After stirring at 80 C for 4 hours under a nitrogen atmosphere and cooling to room temperature, the mixture was filtered through celite and the celite washed thoroughly with ethyl acetate. The filtrate was washed with water and brine, dried over sodium sulfate, filtered and concentrated to dryness. The crude product was purified by column chromatography (ethyl acetate / petroleum ether = 1: 50) to give the title compound (95.1 g, 82.6%) as a brown solid.

The synthetic route of 90347-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Life Sciences Institute; Zhang Zhiyuan; Huang Shaoqiang; Ren Yan; Cui Bo; Cao Weiye; Liu Chunyan; Liu Xiao; (27 pag.)CN107353286; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 58755-70-7, name is 1-Iodo-4-methoxy-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. Formula: C7H6INO3

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 1-Iodo-4-methoxy-2-nitrobenzene 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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, 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. HPLC of Formula: C3H4F3I

110 g (760 mmol) of thiobarbituric acid of formula (XI) was added to 360 mL of water at room temperature,System was suspended state,66.9 g (1.67 mol) of sodium hydroxide was added to the system,The system gradually become clear,Plus,Stir at room temperature for 0.5 h.To the system was added 220 ml of N, N-dimethylformamide,Then 340.4 g (1.52 mol) of 1-iodo-3,3,3-trifluoropropane was added to the system,Plus,Heating to 60 C stirring reaction 8h,TLC monitoring to the basic disappearance of raw materials,The reaction is complete,Stop the reaction,Cooling to room temperature,With 2mol / L hydrochloric acid to adjust the pH to 2.5,filter,Washed cake,After solid drying,Beating,Filtered to give 171.5 g of a white solid,I.e. a compound of formula (X)Yield: 94%

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shandong Bainuo Pharmaceutical Co., Ltd.; Zhen Yizhan; Zhang Zhiqiang; Gao Changsong; Lv Wei; Zhang Zhen; (19 pag.)CN105061431; (2017); B;,
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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C3H4F3I

[0265] A solution of Mg (1.16 g, 1.6 eq.) and I2 (cat.) in Et2O (48 mL) was treated with 3,3,3-trifluoro-1-iodopropane (8.0 g, 1.2 eq. initially 20% of total) and the resulting solution was heated to reflux to initiate Grignard formation. Following initiation, the remaining 3,3,3-trifluoro-1-iodopropane was added dropwise to maintain a gentle reflux. The reaction mixture was stirred at room temperature an additional hour and transferred via canulae to a solution of 4-trifluorobenzaldehyde (4.1 mL, 30 mmol) in Et2O (95 mL) at 0 C. The resulting solution was stirred at 0 C. for 1 hour and room temperature for 1 hour. The reaction was quenched by pouring it over ice (100 g) and saturated NH4Cl. The resulting solution was extracted with CH2Cl2, the combined organics were dried over Na2SO4, filtered, concentrated and used without further purification.

According to the analysis of related databases, 460-37-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Schering Corporation; US2003/232837; (2003); A1;,
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. 135050-44-1, name is 3-Chloro-4-iodoaniline, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

Ethyl 3-(5-(2-(bromomethyl)-4,5-difluorophenyl)picolinamido)propanoate (1.0 g, 2.3 mmol), 3-chloro-4-iodoaniline (1.2 g, 4.7 mmol), and K2CO3 (647 mg, 4.7 mmol) were diluted with DMF (2.4 mL) and the resulting mixture was stirred at room temperature. After 2 h the resulting mixture directly purified via column chromatography to yield the title compound.

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; Chakravarty, Devraj; Kreutter, Kevin; Powell, Mark; Shook, Brian; Song, Fengbin; Xu, Guozhang; Yang, Shyh-Ming; Zhang, Rui; Zhao, Bao-Ping; US2012/302610; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com