Tag: M.W=200-300

Synthetic Route of 645-00-1, 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. 645-00-1, name is 1-Iodo-3-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of aryl halide (0.1mmol) and KOH (0.3mmol), was added to a mixture of DMF (2mL) and ChCl·CuCl (20mol%) under an N2 atmosphere in a round-bottom flask equipped with a condenser. The mixture was heated in an oil bath at 140C and then phenylacetylene (0.15mmol) was added in three portions. The mixture was stirred continuously during the reaction and monitored by both thin-layer chromatography and gas chromatography (GC). After the reaction was complete, the mixture was cooled to room temperature and diluted with EtOAc and H2O. The organic phase was dried over CaCl2, filtered, and concentrated under reduced pressure using a rotary evaporator. The residue was purified by silica gel column chromatography. The products were characterized by IR, 1H NMR, 13C NMR, and GC-MS.

The synthetic route of 1-Iodo-3-nitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hajipour, Abdol R.; Nazemzadeh, Seyed Hadi; Mohammadsaleh, Fatemeh; Tetrahedron Letters; vol. 55; 3; (2014); p. 654 – 656;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 6940-76-7,Some common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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.

4-(3-chloropropyl)-tetrahydro-2H-pyran-4-carbonitrile. To a stirred solution of 1 M LiHMDS (25 mL, 25 mmol) in THF (10 mL) at -78 C. was added dropwise a solution of intermediate 4 (2.23 g, 20 mmol) in THF (15 mL) over 10 minutes. After 40 min, 1-chloro-3-iodopropane (2.7 mL, 25 mmol) was added at once, stirred at -78 C. for 1 h and 4 h room temperature. Then the reaction mixture was diluted with ether (100 mL), washed with water (20 mL) and brine (20 mL), dried (Na2SO4), filtered and concentrated to give yellow oil which was purified by flash column chromatography using 10-30% EtOAc/Hexanes to afford the product intermediate 5 as a colorless liquid (3.737 g, 99%). 1H NMR (500 MHz, CDCl3) delta: 3.97 (2H, dd, J=11.3, 3.7 Hz), 3.71 (2H, td, J=12.2, 1.8 Hz), 3.61 (2H, t, J=6.3 Hz), 2.05-1.98 (2H, m), 1.88 (2H, dd, J=13.4, 1.8 Hz), 1.77-1.74 (2H, m), 1.65-1.59 (2H, m).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chloro-3-iodopropane, its application will become more common.

Reference:
Patent; Naidu, B. Narasimhulu; US2005/256109; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 618-91-7, The chemical industry reduces the impact on the environment during synthesis 618-91-7, name is Methyl 3-iodobenzoate, I believe this compound will play a more active role in future production and life.

General procedure: To an eggplant flask was added H-phosphinate 2a (86.5 mg,0.509 mmol), NiCl2 (7.7 mg, 0.0509 mmol), 2,2`-bipyridine (17.1 mg,0.109 mmol), triethylamine (142 mL, 1.02 mmol), zinc dust (43.2 mg, 0.610 mmol), iodobenzene 1a (68.0 mL, 0.610 mmol) and dry DMF (1.0 mL) under Ar. Then the mixture was stirred at 50 C for 24 h. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/EtOAc 1:1) to give 3a (118 mg, 94%).

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, Methyl 3-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kinbara, Atsushi; Ito, Momoko; Abe, Tohru; Yamagishi, Takehiro; Tetrahedron; vol. 71; 40; (2015); p. 7614 – 7619;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 60577-34-6, These common heterocyclic compound, 60577-34-6, name is 4-Iodo-N-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.

General procedure: A 50 mL round bottom flask was charged with compound 12 (1 equivalent), CuI (0.40.5 equivalents), anhydrous K2CO3 (2-4 equivalents), pipecolinic acid (0.81.0 equivalents) and appropriate iodobenzene (2-3 equivalents). The flask was connected to a vacuum for 3 min, followed by addition of anhydrous DMF using a syringe. The flask was purged with argon for 5 min and then heated in an oil bath maintained at 110 C. On heating, the color of the suspension turned orange/pink, and this color change lasted for about 2 h. The reaction was stirred for an additional 22 h at 110 C. The reaction mixture was then allowed to cool to room temperature. Ethyl acetate (25 mL) was added, and the mixture was poured into water (100 mL). The product was extracted with ethyl acetate (100 mL × 2). The combined organic extracts were washed with brine (100 mL) and dried (anhydrous Na2SO4) and concentrated under reduced pressure. Silica gel (500 mg) was added and the solvent evaporated to obtain a plug, which was purified by column chromatography using hexanes and ethyl acetate (10:1 to 2:1). Fractions containing the product (TLC) were pooled and evaporated to afford 14, 17, and 18 in 27-36% yield.

The synthetic route of 60577-34-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Devambatla, Ravi Kumar Vyas; Choudhary, Shruti; Ihnat, Michael; Hamel, Ernest; Mooberry, Susan L.; Gangjee, Aleem; Bioorganic and Medicinal Chemistry Letters; vol. 28; 18; (2018); p. 3085 – 3093;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 33348-34-4, The chemical industry reduces the impact on the environment during synthesis 33348-34-4, name is 4-Amino-3-iodobenzonitrile, I believe this compound will play a more active role in future production and life.

General procedure: A mixture of 2-iodoanilines (1.0 mmol), THF (3 mL), and t-BuOK (3 mmol) was stirred in a 10-mL sealed Schlenk tube for 5 min, and then dimethylthiocarbamoyl chloride (1.2 mmol) and CuBr (10 mol %) were added. The reaction mixture was heated at 60 C until completion as indicated by TLC. Then the mixture was cooled down to room temperature and quenched with sat. NH4Cl solution (5 mL). The aqueous phase was extracted with EtOAc (3 x10 mL). The combined organic phases were dried (Na2SO4), and the solvent was removed under reduced pressure. The obtained crude product was purified by flash column chromatography.

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, 4-Amino-3-iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chang, Cai-Zhu; Xu, Wan; Zeng, Meng-Tian; Liu, Min; Liu, Xing; Zhu, Hui; Dong, Zhi-Bing; Synthetic Communications; vol. 47; 13; (2017); p. 1262 – 1267;,
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. 4387-36-4, name is 2-Iodobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Iodobenzonitrile

General procedure: To an oven-dried, Ar-flushed Schlenk flask, equipped with a magneticstir bar, was added a solution of Zn species 2 (2.0 mL, 0.5 Min THF, 1.0 mmol, 1.0 equiv). Pd(OAc)2 (4.5 mg, 0.02 mmol, 0.02equiv) and X-Phos (19 mg, 0.04 mmol, 0.04 equiv) were added, followedby aromatic halide substrate 3 (0.7 equiv). The mixture wasstirred at 50 °C for 1 h and then poured into a solution of NH4Cl?EtOAc (25 mL/25 mL). The crude product was separated and the aqphase extracted with EtOAc (3 × 25 mL). The combined organiclayers were dried over MgSO4, filtered and concentrated in vacuo.

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 4387-36-4.

Reference:
Article; Blanc, Romain; Groll, Klaus; Bernhardt, Sebastian; Stockmann, Paul N.; Knochel, Paul; Synthesis; vol. 46; 8; (2014); p. 1052 – 1058;,
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. 620-05-3, name is (Iodomethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., name: (Iodomethyl)benzene

General procedure: A mixture of p-tert-butylcalix[4]arene (1 mmol), potassium carbonate (4 mmol), potassium iodide (20 mol%) in acetonitrile (30 mL) was refluxed at 85 C temperature for 30 min. The reaction mixture was cooled to room temperature and alkyl halide (2.1 mmol) was added to it followed by refluxing (4 mmol for 2m, 2p). The progress of the reaction was monitored byTLC (ethyl acetate/hexane 3:7). After completion, the reaction was cooled to room temperature and the contents were filtered. Solvent was evaporated on a rotary evaporator. The residue obtained was dissolved in chloroform and extracted with water.Chloroform layer was washed with NaCl (brine) and dried over sodium sulfate. Chloroform was evaporated under reduced pressure by using rotary evaporator and the precipitate obtained was recrystallized (chloroform/methanol, 3:7) to afford pure calixarene derivatives.

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 620-05-3.

Reference:
Article; Arora, Lakhbeer Singh; Chawla, Har Mohindra; Shahid, Mohammad; Pant, Nalin; Organic Preparations and Procedures International; vol. 49; 3; (2017); p. 228 – 235;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 4028-63-1,Some common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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 room temperature,A mixture of 2,4,6-trimethyliodobenzene (1.2 mmol, 3 equiv)Elemental selenium (1.2 mmol, 3 equiv),5-phenyl-1,3,4-oxadiazole (0.4 mmol, 1 equiv),Cu (OAc) 2 (0.04 mmol),Potassium carbonate (1.2 mmol, 3 equiv) was added to the reaction tube,Then filled with nitrogen, and replaced three times, in the nitrogen reaction environment,Then, 2 mL of DMF was added to the reaction solvent and stirred at 140 ° C for 24 h.After the reaction was monitored by thin layer chromatography, the reaction mixture was cooled,Then diluted with ethyl acetate, and the diluted solution was transferred to a separatory funnel,Extracted with saturated brine, separated from the aqueous phase and organic phase, and then extracted with ethyl acetate 3 times,The organic phases were combined, 5 g of anhydrous sodium sulfate was added,Wash the filter cake with 5 mL of ethyl acetate each time 3 times, then spin off the solvent,The product was isolated by column chromatography (eluent: petroleum ether: ether = 98: 2)The product was a yellow solid, yield 90percent, product weight 123 mg.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou Medical University; Wu Ge; (23 pag.)CN107056727; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

847685-01-2, name is 4,5-Difluoro-2-iodoaniline, 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. Formula: C6H4F2IN

General procedure: Pd(PPh3)2Cl2 (28 mg, 0.04 mmol), CuI (17 mg, 0.09 mmol) and Et3N (3mL) were added to a stirred solution of iodoaniline 2(b-f) or 2-iodoaniline (7) (1 mmol), 2-methylbut-3-yn-2-ol (126 mg, 1.5 mmol) in dry MeCN (10mL) at room temperature under an argon atmosphere. The mixture was heated at 50C for 2 h with stirring. The reaction mixture was allowed to cool down to room temperature, and CH2Cl2 (10 mL) was added. The mixture was poured into H2O (40 mL) and extracted with CH2Cl2 (3× 50mL). The combined organic layers were washed with H2O (40 mL) and dried (MgSO4). The evaporation of the solvent in vacuo gave the crude product 3(b-f) or 4-(2-aminophenyl)-2-methylbut-3-yn-2-ol (8) that was used without further purification (the 1H and 19F NMR spectra agreed with the literature data [11,12]).

The synthetic route of 847685-01-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Politanskaya, Larisa V.; Chuikov, Igor P.; Tretyakov, Evgeny V.; Shteingarts, Vitalij D.; Ovchinnikova, Ludmila P.; Zakharova, Olga D.; Nevinsky, Georgy A.; Journal of Fluorine Chemistry; vol. 178; (2015); p. 142 – 153;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 123158-75-8,Some common heterocyclic compound, 123158-75-8, name is 4-Chloro-2-iodo-6-nitroaniline, molecular formula is C6H4ClIN2O2, 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 1)2-Iodo-4-chloro-6-nitro-phenylamine (10.0 g, 33.50 mmol) of was dissolved in 200 ml of tetrahydrofuran, and 3.97 g (50.25 mmol) of pyridine and 7.74 g (36.85 mmol) of trifluoroacetic anhydride were added. The mixture was stirred for 9 hours at 0 C.room temperature. At the end of reaction, the reaction mixture was diluted with water and extracted with ethylacetate. The extract was washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and separated by column chromatography to obtain trifluoroacetamide 12.3 g (Yield 85%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Chloro-2-iodo-6-nitroaniline, its application will become more common.

Reference:
Patent; Kim, Soon Ha; Kim, Hyoung Jin; Chung, Chul Woong; Park, Heui Sul; Kwak, Hyo Shin; Kim, Sung Ho; Park, Jin Gu; US2010/291533; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com