Category: iodides-buliding-blocks

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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-4-iodo-2-methoxybenzene

(2E)-3-(4-Bromo-3-methoxyphenyl)acrylic acid 119 To a solution of 1-bromo-4-iodo-2-methoxybenzene (L. A. Hasvold et al., US 2004/0254159) in MeCN (1.1 M) was added acrylic acid (1.24 eq.), TEA (2.5 eq.) and palladium acetate (0.03 eq). The reaction mixture was heated to 90 C. for 40 min, cooled to RT and poured into 1N HCl. After sting for 30 min, the solid was filtered, heated to reflux in EtOH (2.3 M), allowed to cool to RT and stirred overnight. The solid was filtered and washed with 1:1 EtOH:hexane to give the desired product 119. LRMS ESI+ (M+H)+ 257.0.

The synthetic route of 755027-18-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Istituto di Ricerche di Biologia Molecolare P. Angeletti SPA; US2009/312241; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 755027-18-0, The chemical industry reduces the impact on the environment during synthesis 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, I believe this compound will play a more active role in future production and life.

Acrylic acid (9.61 g, 133 mmol), TEA (37.2 mL, 267 mmol) and palladium acetate (719 mg, 3.2 mmol) were added to a solution of 1-bromo-4-iodo-2-methoxybenzene () (33.45 g, 107 mmol) in MeCN (100 mL). The reaction mixture was heated to 90C for 40 min, cooled to RT and poured into 2.4 L 1M HCl. After stirring for 30 min, the solid was filtered, heated to reflux in EtOH (230 mL), allowed to cool to RT and stirred overnight. The solid was filtered and washed with 1:1 EtOH:hexanes (50 mL) to give desired product. LRMS ESI+ (M+H)+ 257.0.

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-Bromo-4-iodo-2-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Merck Sharp & Dohme Corp.; MSD Italia S.r.l.; MCCAULEY, John, A.; LIVERTON, Nigel, J.; HARPER, Steven; MCINTYRE, Charles, A.; RUDD, Michael, T.; (73 pag.)EP2268285; (2018); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 103440-52-4, The chemical industry reduces the impact on the environment during synthesis 103440-52-4, name is Methyl 2-Iodo-5-methylbenzoate, I believe this compound will play a more active role in future production and life.

Methyl 5-methyl-2~(4 A5.54etramethyl- 1 ,3.2-dioxaborolan-2-yDbenzoate (B-2)A solution of B4 (5.9 kg, 21.37 mol) in iPAc was charged in a visually clean 100 L reactor equipped with a mechanical stirrer and thermocouple. The solution was solvent switched to 2-MeTHF (-35 L). Triethylamine (8.94 L5 64.1 mol) was added and the solution was degassed with N2- Pinacol borane (4.65 L, 32.1 mol) was added slowly (over 15 mins) to the stirring solution while maintaining the purge. The solution was further degassed for 10 min and tri-o-tolylphosphine (0.325 kg, 1.069 mol) was added followed by palladium (II) acetate (0.120 kg, 0.534 mol). This caused the reaction to turn black immediately with a slow exotherm from 11.5 0C to 30 0C. At this point a delayed exotherm was observed and the reaction temperature increased to 60 0C (over 45 min). The reaction temperature was increased to 77 0C and aged for another 45 min. At this point, HPLC analysis of a reaction aliquot revealed complete consumption of the starting material. The heat source was removed and an ice bath was placed under the flask to cool the reaction over 1.5 h. A 26 w% ammonium chloride solution was added very slowly to control gas evolution and exotherm (over 60 minutes) which caused a black precipitated to form. The supernatant was transferred to an extractor which already contained 40 L of water. The black slurry remaining was filtered on Solka-Floc and washed with MTBE (-20 L). The filtrate was loaded into the extractor. The layers were cut and assay of the organic layers revealed R-2 (4.45 kg, 16.11 mol, 75 % yield) in 81.6% purity and was used as is in the following step. lH NMR (500 MHz, CDC13, 293K, TMS); 7.75 (1 H, s), 7.40 (1 H, d, J = 7.49 Hz), 7.32 (1 H, d, J = 7.56 Hz)5 3.90 (3 H, s), 2.37 (3 H5 s), 1.41 (12 H5 s).

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 2-Iodo-5-methylbenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; MERCK FROSST CANADA LTD.; WO2009/143033; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 108078-14-4, name is 2-Iodo-3-methylbenzoic acid, molecular formula is C8H7IO2, 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. Product Details of 108078-14-4

General procedure: A mixture of 2-iodobenzoic 1a (0.2 mmol), acetylacetone 2a (0.4 mmol), and Cs2CO3 (65.2 mg, 0.20 mmol) in CH3CN was stirred at 100 C. When the reaction was considered complete as determined by TLC analysis, the reaction was allowed to cool to room temperature and quenched by water, and the mixture was extracted with CH2Cl2. The combined organic extracts were washed with water and saturated brine. The organic layers were dried over Na2SO4, filtered. Solvents were evaporated under reduced pressure. The residue was purified by chromatography on silica gel to afford isocoumarins derivatives and isoquinolone derivatives.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108078-14-4, its application will become more common.

Reference:
Article; Liu, Lei; Hu, Jie; Wang, Xiang-Chuan; Zhong, Mei-Jin; Liu, Xue-Yuan; Yang, Shang-Dong; Liang, Yong-Min; Tetrahedron; vol. 68; 27-28; (2012); p. 5391 – 5395;,
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. 618-91-7, name is Methyl 3-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H7IO2

General procedure: To a mixture of Iodobenzene (1.0 mmol), styrene (1.2 mmol), NaOAc (1.5 mmol), Catalyst (0.007 mmol) and DMF (3mL) was added in round bottom flask. (No inert gas protection was needed.). The reaction was carried out at 120 C for 15 min. Upon completion of reaction as indicated by TLC, the reaction mixture was poured in crushed ice-water, extracted with ethyl acetate, dried over anhydrous Na2SO4, concentrated in vacuum to give crude product which was purified through column chromatography on silica gel (100-200) to afforded pure stilbenes in 90-98% yields.

The synthetic route of 618-91-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sharma, Sonam; Sarkar, Bibhas R.; Synthetic Communications; vol. 48; 8; (2018); p. 906 – 914;,
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. 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, A new synthetic method of this compound is introduced below., Computed Properties of C13H7F3INO2

1 , 1 -Dimethylethyl 3 -hydroxy-3 -(2-methyl- 1 -nitropropyl)azetidine- 1 -carboxylate (105 mg, 0.38 mmol) was taken into methanol (1 mL) followed by addition of 4 N anhydrous hydrogen chloride in dioxane (1 mL) and the acidic solution was allowed to stand for 15 minutes at room temperature then concentrated and dried in vacuo to an amorphous residue. 3,4-Difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (150 mg, 0.38 mmol), prepared using procedures similar to those described in US 7,019,033, was taken into DMF (0.7 mL) followed by addition of PyBOP (198 mg, 0.38 mmol) and the solution was allowed to stir for 10 minutes at room temperature. The above amine hydrochloride salt and DIPEA (190 muL, 1.1 mmol) in DMF solution (0.7 mL) was added and the mixture was allowed to stir for one hour at room temperature. The mixture was partitioned with ethyl acetate and 0.5 N aqueous EPO hydrochloric acid and the organic phase washed three times with water then brine and dried over anhydrous magnesium sulfate. Filtration and concentration afforded a residue that was further purified by silica gel flash chromatography using 1.5:1 hexanes:ethyl acetate as eluent to give l-({3,4-difluoro-2-[(2-fluoro-4-iodophenyl)amino]phenyl}carbonyl)-3-(2-methyl-l- nitrorhoropyl)azetidin-3-ol (189 mg, 90% yield) as an amorphous solid. 1H-NMR (400 MHz, CDCl3): 8.41 (br s, IH), 7.41 (dd, IH), 7.34 (d, IH), 7.09 (br m, IH), 6.81 (q, IH), 6.65-6.60 (m, IH), 4.49 (d, IH), 4.15-4.09 (m, 4H), 3.66 (s, IH), 2.56-2.46 (m, IH) 1.03 (d, 6H).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EXELIXIS, INC.; WO2007/44515; (2007); 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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, A new synthetic method of this compound is introduced below., Safety of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

2.4. Synthesis of 1-chloro-3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin (Cl-FODMH)3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin (FODMH)was synthesized using similar procedures as in the preparation ofODMH. Briey, 3.20 g DMH were dissolved in 30 mL methanol inthe presence of 1.68 g potassium hydroxide. The mixture was keptat 50 C for 30 min. After evaporation of the solvent, the potassiumsalt of DMH was dried in a vacuum oven at 60 C for three days. Theanhydrous salt was then dispersed in 100 mL N,N-dime-thylformamide (DMF) at 95 C for 10 min under constant stirring,after which 11.85 g IFO were added into the mixtures. The reactionwas continued for 4 h at 95 C. At the end of the reaction, theformed KI was ltered off. After the removal of DMF by distillationunder reduced pressure, the residual substance was recrystallizedfrom ethanol. 3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin(FODMH) was obtained as white powders with a yield of 60.7%(7.22 g).In the preparation of Cl-FODMH, 0.5 g FODMH and 0.74 g tri-chloroisocyanuric acid (TCCA) were dissolved in acetone [10]. Here,TCCA was employed because our screening tests showed that usingchlorine bleach as the chlorination agent could not chlorinateFODMH successfully due to the very hydrophobic nature ofFODMH. The solution was vigorously stirred for 30 min at ambienttemperature. At the end of the reaction, acetone was evaporated,hexane was added to the mixtures, and the insoluble solids wereltered off. After removing hexane from the ltrate by evaporation,Cl-FODMH was obtained as white powders with a yield of 59.2%.

The synthetic route of 2043-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lin, Jiajin; Jiang, Fuguang; Wen, Jianchuan; Lv, Wei; Porteous, Nuala; Deng, Ying; Sun, Yuyu; Polymer; vol. 68; (2015); p. 92 – 100;,
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. 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid

A solution of 3,4-difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (200 mg, 0.51 mmol), prepared using procedures similar to those in US 7,019,033, PyBOP (256 mg, 0.51 mmol), commercially available tert-butyl azetidin-3-ylcarbamate (131 mg, 0.77 mmol) and lambdazetaiV-diisopropylethylamine (180 muL, 1.02 mmol) in dimethylformamide (3 mL) was stirred at room temperature for 15 hours. The reaction mixture was partitioned between 5% aqueous lithium chloride and ethyl acetate. The organic portion was washed with 20% aqueous citric acid, saturated aqueous sodium bicarbonate, brine, dried over sodium sulfate, filtered and concentrated in vacuo to afford a brown residue which was purified by silica gel column chromatography eluting with 30% ethyl acetate in hexanes to afford 1,1- dimethylethyl [ 1 -( { 3 ,4-difluoro-2- [(2-fluoro-4-iodophenyl)amino]phenyl } carbonyl)azetidin- 3-yl]carbamate (225 mg, 80% yield) as a colorless oil. 1H NMR (400 MHz, DMSO): 8.56 (s, IH), 7.60-7.55 (m, 2H), 7.38 (d, IH), 7.30-7.26 (m, IH), 7.20-7.13 (m, IH), 6.71-6.66 (m, IH), 4.37-4.20 (m, 2H), 4.18-4.06 (m, IH), 3.98-3.93 (m, IH), 3.82-3.75 (m, IH), 1.37 (s, 9H). MS (EI) C2IH21N3O3F3I: 548 (MH+).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EXELIXIS, INC.; WO2008/124085; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 626-44-8 as follows. Recommanded Product: 1,3,5-Triiodobenzene

Synthesis of 1 , 3 , 5-tris [( 1 , 3-diethylcarboxylate-5- ( 4- (ethynyl ) phenyl )) butadiynyl ] -benzene (compound 6). 1,3,5- Triiodobenzene (5, 1.1 g, 2.41 mmol), compound 4 (3.0 g, 11.1 mmol), THF (100 ml), and diisopropylamine (50 ml) are combined in a 500 mL Schlenk flask equipped with a magnetic stir bar and a rubber stopper. The mixture is cooled to -78 °C in an acetone/dry ice bath and subjected to three cycles of brief vacuum-degas/N2 back-fill with no stirring. Then Pd(PPh3)4 (450 mg, 0.39 mmol) and Cul (150 mg, 0.79 mmol) is added to this degassed solution under positive N2 flow and the mixture is degassed for three more cycles. The solution is stirred for 48 h at 25 °C, concentrated, and dried under high vacuum. The remaining brown paste is redissolved in a minimum amount of CHCI3, and column chromatographed over silica gel using CHCI3 (stabilized with 2percent ethanol) to give a brown solid (2.1 g) , which is recrystallized three times from CHCl3:EtOH (75 ml, 2:1, v/v) to give the product 6 as an off-white solid. Yield = 1.7 g (80percent). XH NMR (500 MHz, CDC13) is shown in Fig. 16, where delta 1.42 (t, J = 7.0 Hz, 18H, -C02CH2C) , 4.43 (q, J = 7.0 Hz, 12H, -C02Cfi2CH3) , 7.65 (s, 3H, Ar2-fi) , 8.35 (d, J = 1.5 Hz, 6H, Ari-H) , 8.67 (t, J = 1.5 Hz, 3H, Ari-H) . 13C NMR (126 MHz, CDCI3) is shown in Fig. 17, where delta 14.43, 61.88, 75.13, 75.50, 79.78, 80.63, 122.45, 123.00, 131.29, 131.60, 136.72, 137.36, and 164.92.

According to the analysis of related databases, 626-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NORTHWESTERN UNIVERSITY; FARHA, Omar, K.; HUPP, Joseph, T.; WILMER, Christopher, E.; ERYAZICI, Ibrahim; SNURR, Randal, Q.; GOMEZ-GUALDRON, Diego, A.; BORAH, Bhaskarjyoti; WO2013/192146; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 249647-24-3, name is Methyl 3-bromo-4-iodobenzoate, molecular formula is C8H6BrIO2, 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: Methyl 3-bromo-4-iodobenzoate

Example 31Preparation of lambda/-r2-amino-1-(phenylmethyl)ethyll-3-bromo-4-(1-methyl-1/-/-pyrazol- 5-yl)benzamidea) methyl 3-bromo-4-(1-methyl-1 /-/-pyrazol-5-yl)benzoateTo a solution of methyl 3-bromo-4-iodobenzoate (409 mg, 1.2 mmol) in dioxane/H2O (4:1 , 10 ml.) was added K2CO3 (497 mg, 3.6 mmol), tetrakistriphenylphosphine Pd(O) (69 mg, 0.06 mmol) and 5-(5,5-dimethyl-1 ,3,2- dioxaborinan-2-yl)-1-methyl-1 /-/-pyrazole (349 mg, 3.6 mmol). The reaction mixture was heated to 80 C in a sealed tube for 12h and was then partitioned between 6N NaOH and DCM. The pH of the aqueous phase was adjusted to ~3 with 3M HCI and washed several times with DCM. The combined organic fractions were dried (Na2SO4), concentrated under vacuum and used directly without further purification (307 mg, 87%): LC-MS (ES) m/z = 296 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 249647-24-3, its application will become more common.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2008/121786; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com