Month: June 2021

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. 2974-94-9, name is 1-Iodo-4-phenoxybenzene, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

General procedure: A 10 mL flask was charged with a magnetic stir bar, CuI (19 mg,10 mol%), L2 (86 mg, 20 mol%), Cs2CO3 (651 mg, 2 mmol) and solid aryl iodides (1.0 mmol). The tube was evacuated and backfilled with argon (this procedure was repeated three times). Under a counter flow of Argon, DMSO (1.0 mL), 1.0 mmol aryl iodides (if liquid), 0.9 mL (12.0 mmol) aqueous ammonia (28%) were added by syringe slowly. The reaction mixture was allowed to stir under argon at room temperature for 24 h. Then the mixture was diluted with 30 ml dichloromethane and passed through a fritted glass filter, the filter cake being further washed with 15 ml dichloromethane, dried over Na2SO4, filtered and the most solvent was removed under vacuum. The residue was purified by column chromatography on silica gel with an eluent of petroleum ether and ethyl acetate.

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:
Article; Chen, Dong; Dong, Xinrui; Jiang, Shang; Jiang, Sheng; Qiu, Yatao; Wu, Xiaoxing; Tetrahedron Letters; (2020);,
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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, A new synthetic method of this compound is introduced below., Quality Control of Methyl 5-bromo-2-iodobenzoate

A magnetically stirred and degassed mixture of compound 5 (1.39 g, 20.8 mmol), compound 37 (6.45 g, 18.9 mmol), Cul (359 mg, 1.9 mmol), 1 , 10-phenanthroline (680 mg, 3.8 mmol) and Cs2C03 (9.30 g, 28.4 mmol) in anhydrous toluene (40 mL) was heated at 100 C under a nitrogen atmosphere for 48 h. The cooled reaction mixture was then passed through a pad of TLC-grade silica and the filtrate concentrated under reduced pressure. The residue so formed was subjected to flash chromatography (silica, 30: 1 v/v hexane/ethyl acetate elution) to afford, after concentration of the appropriate fractions (Rf = 0.5 in 8: 1 v/v hexane/ethyl acetate), compound 38 (5.21 g, 99%) as a clear, colorless syrup. (0734) 1H NMR (400 MHz, CDCI3) £ 7.85 (d, J = 2.4 Hz, l H), 7.59 (dd, J = 8.5 and 2.4 Hz, 2H), 7.18 (m, 1H), 6.71 (m, 2H), 6.25 (m, 2H), 3.65 (s, 3H). (0735) 13C NMR (100 MHz, CDC13) delta 166.1 , 139.4, 135.3, 133.5, 129.4, 128.3, 122.0, 120.5, 1 10.2, 52.8. (0736) IR vmax 2950, 1729, 1594, 1563, 1498, 1435, 1400, 1329, 1288, 1267, 1238, 1 123, 1094, 1015, 966, 922, 826, 727 cm 1. (0737) MS (ESI, +ve): m/z 282 and 280 [(M+H) , both 50%], 250 and 248 (96 and 100). (0738) HRMS (ESI, +ve) Found: (M i l ) . 279.9972. C12Hi179BrN02 requires (M i l ) . 279.9973.

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; THE AUSTRALIAN NATIONAL UNIVERSITY; BANWELL, Martin Gerhardt; ZHANG, Yiwen; (159 pag.)WO2017/100819; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 869500-07-2, 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. 869500-07-2, name is 1-Bromo-2-iodo-3-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a souton of 5(4,455tetramethy-1 (nterrnedafte28, 250 mg, 0.96 mmo), potassum phosphate (408 mg, 1.9 mmo), and 1-bromo–2odo3 methybenzene (342 mg, 1.1 mmo) ri 4:1 doxane:water (6.6 mL) was added PdC2(dppf)- CH2C2 (35 mg, 0.05 mmo) at once. The mixture was degassed with n[trogen for 10 minutes and then heated at 100 C for 16 h. After coong to rt, the reacUon nixture was duted w[th water and extracted with DCM (x3). The combned organc extracts were dried(NaSO), fl[tered and concentrated under reduced pressure. The crude product was purfled by flash coumn chromatography (SO2; 0 5% DCM/MeOH) to provide the tWe compound as a wh[te sod (98 mg, 34% yed).. MS (ES): mass cacd. for C14H11BrN2O, 3020; m/zfound, 303.1 [M+Hj. 1H NMR (400 MHz, DMSOd6) oe 1069 (s, IH), 10.65 (5, 1H), 7.53 (dt, J= 8.0, 0.9 Hz, IH), 7.30(dt, J= 7.5, 1.1 Hz, IH), 7.23-7.12 (m, 1H), 6.99(d, J = 7.9 Hz, 1 H), 6.73 6.61 (m, 2H), 2.04 (s, 3H).

The synthetic route of 1-Bromo-2-iodo-3-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; RAVULA, Suchitra; SWANSON, Devin M.; SAVALL, Bradley M.; AMERIKS, Michael K.; (250 pag.)WO2016/176449; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 20555-91-3, 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. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The air was exchanged 3 times with nitrogen in a 25 mL test tube reactor. The first step was to first substrate 1a (0.2 mmol, 57.1 mg), pinacol borate (0.4 mmol, 102 mg), Pd (PPh3) 4 (0.02 mmol, 23.1 mg), cesium carbonate (0.4 mmol, 130 mg) Weighed into the reaction tube, vacuumed for nitrogen, and added tetrahydrofuran (2 mL) and water (0.014 mL) under nitrogen, and the reaction was heated to 60 C for 12 hours; the second step was added for 2 hours ( 0.24 mmol,65.5 mg) continued to react at this temperature for 12 hours. After TLC detects the reaction,The system was cooled to room temperature. Directly add silica gel, spin dry column chromatography,Obtained a reddish brown solid 3ah (41%).

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, 1,2-Dichloro-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shandong University of Technology; Liu Hui; Cui Jie; Meng Long; Chi Xiaochen; Sun Xi; Cao Chengqiang; Liu Qing; Li Xinjin; Zhou Zhen; Dong Yunhui; (16 pag.)CN109553555; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 147808-02-4, 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 147808-02-4 as follows.

Example 11 5-Chloro-N-((1-(2-fluoro-4-(2-oxopyridin-1(2H)-yl)phenyl)-1H-imidazol-4-yl)methyl)thiophene-2-carboxamide (21) A mixture of 2,5-diiodofluorobenzene II-4 (2.00 g, 5.75 mmol), 2-hydroxypyridine 1-7 (0.546 g, 5.75 mmol), 8-hydroxyquinoline (0.083 g, 0.57 mmol) and K2CO3 (1.00 g, 7.25 mmol) in DMSO (10 mL) was degassed before being charged with CuI (0.109 g, 0.57 mmol). The mixture in a sealed tube was heated at 130 C. overnight. Water and EtOAc were added. The mixture was filtered. The organic layer was separated, then applied to a silica gel column, which was eluted with 0-70% EtOAc in hexane to give 1-iodo-2-fluoro-4-(2-oxopyridin-1(2H)-yl)benzene 3-2 (0.820 g). MS 315.8 (M+H).

According to the analysis of related databases, 147808-02-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Millennium Pharmaceuticals, Inc.; US2007/259924; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 618-91-7, name is Methyl 3-iodobenzoate, 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 618-91-7, Quality Control of Methyl 3-iodobenzoate

General procedure: An oven-dried Schlenk tuble equipped with a magnetic stirring bar was charged with MCM-41-N,N-Pd(OAc)2 (49 mg, 0.02 mmol Pd), aryl iodide (3.2 mmol), triarylbismuth (1.0 mmol), and K2CO3 (4.0 mmol) followed by anhydrous NMP (3 mL) under Ar. The reaction mixture was stirred in an oil bath at 110 C for 5-24 h. The reaction mixture was cooled to room temperature and filtered. The MCM-41-N,N-Pd(OAc)2 complex was washed with distilled water (2×5 mL), NMP (2×5 mL) and Et2O (2×5 mL) and reused in the next run. The filtrate was quenched with water, and extracted with ethyl acetate (2×30 mL). The combined ethyl acetate extract was washed with dilute hydrochloric acid (10 mL), saturated sodium bicarbonate solution (10 mL), brine (2×10 mL), and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the residue was purified by flash column chromatography on silica gel.

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; Xu, Caifeng; Yin, Lin; Huang, Bin; Liu, Haiyi; Cai, Mingzhong; Tetrahedron; vol. 72; 17; (2016); p. 2065 – 2071;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 51628-12-7, A common heterocyclic compound, 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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 stirred mixture of 4-iodophenylacetonitrile (35), arylboronic acid (36-45) (1.1 equiv), Pd(PPh3)4 (0.03 equiv), KBr (1.1 equiv), and K3PO4 (2.5 equiv) in dioxane (5 mL/mmol) was purged with N2 for10 min at room temperature and then stirred overnight at 85 C under N2. The mixture was diluted with water and extracted with AcOEt. The organic phase was washed three times with water, dried (Na2SO4), and evaporated under vacuum. The residue was chromatographedon silica gel.

The synthetic route of 51628-12-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ortar, Giorgio; Morera, Enrico; De Petrocellis, Luciano; Ligresti, Alessia; Schiano Moriello, Aniello; Morera, Ludovica; Nalli, Marianna; Ragno, Rino; Pirolli, Adele; Di Marzo, Vincenzo; European Journal of Medicinal Chemistry; vol. 63; (2013); p. 118 – 132;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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 10 mL flask equipped with a Teflon valve was charged with a magnetic stir bar, CuI (2 mg, 1molpercent), Heteroarylamine (1.5 mmol), KOtBu (224 mg, 2.0 mmol), solid aryl halides (1.0 mmol). The tube was evacuated and backfilled with argon. Under a counter flow of argon, dioxane (1.5mL), aryl halides (1.0 mmol, if liquid) were added by syringe. The tube was sealed. The reaction mixture was allowed to stir at 110 °C (X=I) or 130 °C (X= Br) for 24 h. Then the mixture was cooled to room temperature and added 5.0 mL brine. Subsequently, the mixture was extracted with ethyl acetate. The organic layers were collected, dried over Na2SO4, filtered and the solvent was removed under vacuum. The residue was purified by column chromatography on silica gel.

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

Reference:
Article; Wang, Deping; Kuang, Daizhi; Zhang, Fuxing; Liu, Yang; Ning, Shunhua; Tetrahedron Letters; vol. 55; 51; (2014); p. 7121 – 7123;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. name: 3-(4-Iodophenyl)propanoic acid

3-(4?-Iodophenyl)propanoic acid (10 mmol, 2.76 g, 1.0 eq.) and N- hydroxysuccinimide (15 mmol, 1.73 g, 1.5 eq) were dissolved in anhydrous CH2Cl2 (40 mL). The mixture was cooled to 0 C, and N,N’-dicyclohexylcarbodiimide (DCC, 15 mmol, 3.09 g, 1.5 eq) dissolved in 20 mL CH2Cl2 was added dropwise slowly. The mixture was stirred overnight at room temperature. The N,N’-dicyclohexylurea was filtered out, the residue was washed with CH2Cl2, and the filtrate was evaporated to dryness purified by column chromatography and recrystallization with iso-propanol or toluene/hexane to afford succinimide as white solid (3.50 g, 94%).1HNMR (400 MHz, CD3CN) delta 7.66 (d, J = 8.4 Hz, 2 H), 7.08 (d, J = 8.4 Hz, 2 H), 2.95 (A2B2, t, 4 H), 2.75 (s, 4 H).13CNMR (100 MHz, CD3CN) delta 168.4, 166.7, 138.1, 135.9, 129.2, 89.5, 30.1, 27.8, 23.8; HRMS (ESI) Calcd for C13H12NO4INa (M+Na)+ : 395.9709;

The synthetic route of 1643-29-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NUTECH VENTURES; DIMAGNO, Stephen; HU, Bao; (36 pag.)WO2016/201125; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 622-50-4, The chemical industry reduces the impact on the environment during synthesis 622-50-4, name is N-(4-Iodophenyl)acetamide, I believe this compound will play a more active role in future production and life.

[Rh(cod)(MeCN)2]BF4 (11.0 mg, 0.0300 mmol, 0.0300 equiv) and 4-iodoacetanilide (260 mg, 1.00 mmol, 1.00 equiv) were charged in 10 mL vial capped with a rubber septum. The vial was evacuated and backfilled with nitrogen. To this vial, DMF (4 mL), triethylamine (0.420 mL, 3.00 mmol, 3.00 equiv) and triethoxysilane (0.360 mL, 2.00 mmol, 2.00 equiv) were added. The reaction mixture was stirred at 80 C for 2 h, then cooled to 23 C. The mixture was diluted with ether (50 mL) and washed three times with water (3×20 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by Kugelrohr distillation to give 238 mg of the title compound as a colorless oil (80% yield). Rf=0.25 (hexanes/EtOAc 1:1 (v/v)). NMR spectroscopy: 1H NMR (500 MHz, CDCl3, 23 C, delta): 7.69 (d, J=8.0 Hz, 2H), 7.59 (d, J=8.5 Hz, 2H), 7.42 (br s, 1H), 3.85 (q, J=7.0 Hz, 6H), 2.17 (s, 3H), 1.23 (t, J=7.0 Hz, 9H). 13C NMR (125 MHz, CDCl3, 23 C, delta): 168.4, 139.8, 135.8, 126.3, 118.9, 58.7, 24.7, 18.2.

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, N-(4-Iodophenyl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Tang, Pingping; Ritter, Tobias; Tetrahedron; vol. 67; 24; (2011); p. 4449 – 4454;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com