Month: September 2021

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. 811842-30-5, name is 2-Bromo-1-fluoro-4-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 811842-30-5

General procedure: To a 20 mL vial with a stir bar was added aryl halide 1 (2.00 mmol), Pd(dba)2 (28.8 mg, 2.5 mol %), Xantphos (28.9 mg, 2.5 mol %). The vial was sealed with a Teflon-lined cap and THF (6.0 mL) was added. The mixture was vacuumed and backfilled with nitrogen (3×). A solution of ethyl 2-bromozincacetate (2a) in THF (0.40 M, 6.0 mL, 1.2 equiv) filtered through a Target Nylon 0.45 mum filter (1.25-inch OD) was syringed in and the reaction mixture was then heated to 65 C and monitored by HPLC. Upon reaction completion based on HPLC analysis (?95% conversion unless the reaction was stalled), the mixture was cooled to room temperature and quenched with 1 M aq HCl (5.0 mL), followed by addition of brine (5.0 mL). The organic layer was separated and concentrated in vacuum. The residue was purified by silica gel column chromatography using gradient EtOAc in hexanes.

The synthetic route of 811842-30-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wong, Brian; Linghu, Xin; Crawford, James J.; Drobnick, Joy; Lee, Wendy; Zhang, Haiming; Tetrahedron; vol. 70; 7; (2014); p. 1508 – 1515;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 2468-56-6, name is 6-Iodohex-1-yne, 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 2468-56-6, Formula: C6H9I

To a solution of diisopropylamine (0.86 mL, 6.1 mmol) in anhydrous THF (10 mL) at 0 C was added n-butyllithium (2.5M in hexane) under nitrogen to give a light yellow solution which was stirred at room temperature for 10 mm. Ethyl 2-(1,3,5-trimethyl-1 H-pyrazol-4- yl)acetate (1.00 g, 5.10 mmol) was added at -78 C and the yellowish orange mixture was stirred at -78 C for 1 hr. 6-iodo-1-hexyne (0.78 mL, 5.9 mmol) was added to give orange mixture which was stirred at -78 C for another I hr before the addition of I ,3-Dimethyl- 3,4,5,6-tetrahydro-2(1 H)-pyrimidinone (DMPU). The mixture was slowly warmed to 0 C in 1 hr and water (5 mL) was added to quench the reaction. Ethyl acetate (3x 200 mL) was used to extract the product and the organic layer was washed with saturated aqueous ammonium chloride solution (20 mL), hydrochloric acid (IM, 20 mL), saturated aqueous sodium carbonate solution (20 mL), brine (20 mL), dried over MgSO4 and concentrated in vacuo to give an orange liquid. The crude product was purified by flash column chromatography by elution with 50% ethyl acetate in hexane to give Ethyl 2-(1 ,3,5-trimethyl-1 H-pyrazol-4-yl)oct- 7-ynoate as a pale yellow oil (233 mg, 17%). ESI HRMS, found 277.1919 (C16H25N202), MW, requires 277.1916. 1H NMR (COds, 400 MHz, 300 K) 64.12-4.01 (2H, m), 3.66 (3H, s), 3.37 (1H, dd, J = 8.4, 7.1 Hz,), 2.17 (6H, d, J = 3.8 Hz), 2.13 (2H, td, J = 7.1, 2.5 Hz), 2.07-1.97 (1 H, m), 1.89 (1 H, t, J 2.6 Hz), 1.73-1.64 (1 H, m), 1.54-1.46 (2H, m,), 1.35-1.27 (2H, m), 1.18 (3H, t, J= 7.1 Hz, Hk).

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, 6-Iodohex-1-yne, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; IMPERIAL INNOVATIONS LIMITED; BELL, Andrew Simon; TATE, Edward William; LEATHERBARROW, Robin John; HUTTON, Jennie Ann; BRANNIGAN, James Antony; (213 pag.)WO2017/1812; (2017); A1;,
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

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

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

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. 41252-96-4, name is 2-Chloro-1-iodo-4-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 41252-96-4

General procedure: A mixture of aryl halide (1.0 mmol), PdCl2 (0.05 mmol), PPh3 (0.10 mmol), CuI (0.1 mmol) and K2CO3 (2.0 mmol) was stirred in H2O (5 mL) at room temperature under an argon atmosphere. 2-Chloro-3-propargylaminoquinoxaline (2) (1.20 mmol) was added, and the mixture stirred at 70 C for 12 h. After completion of the reaction, the resulting solution was concentrated in vacuo, and the crude residue subjected to column chromatography (silica gel) using CHCl3-CH3OH (98:2) as an eluent to afford the pure product (Table 1).

The synthetic route of 41252-96-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bakherad, Mohammad; Keivanloo, Ali; Samangooei, Shahrzad; Tetrahedron Letters; vol. 53; 12; (2012); p. 1447 – 1449;,
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. 2786-00-7, name is 5-Iodo-2-methoxybenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-Iodo-2-methoxybenzoic acid

5-iodo-2-methoxybenzoic acid (2.0 g, 7.2 mmol) was suspended in anhydrous dichloromethane (40 ml). To this suspension was added, with stirring under nitrogen, oxalyl chloride (0.754 ml, 8.62 mmol). N,N-dimethylformamide (0.035 ml) was then added dropwise to the reaction mixture, and the mixture stirred for 1 hour at room temperature. When the intermediate acid chloride was fully formed as demonstrated by LC/MS, isopropanol (20 ml) was slowly added, then after 15 minutes solid sodium bicarbonate (2 g) was slowly added. The reaction was diluted with 40 ml of 1:1 saturated sodium bicarbonate and water, and the aqueous phase extracted with dichloromethane (3*40 ml). The organic extracts were combined, dried over magnesium sulfate, and solvent removed under reduced pressure. The residue was purified by column chromatography (0 to 50% ethyl acetate in hexanes) to afford isopropyl 5-iodo-2-methoxybenzoate as an oil (1.6 g, 5.0 mmol). 69% yield. 321 (M+1).

According to the analysis of related databases, 2786-00-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Gilead Sciences, Inc.; US2012/4267; (2012); 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. 450412-29-0, name is 1-Bromo-3-fluoro-2-iodobenzene, A new synthetic method of this compound is introduced below., name: 1-Bromo-3-fluoro-2-iodobenzene

Bromo-3-fluoro-2-iodobenzene (100 g, 333.5 mmol), 5-chloro-2-methoxyphenylboronic acid 2-methoxyphenyl) boronic acid (62.2 g, 333.5 mmol) was dissolved in 800 ml of tetrahydrofuran (THF). A solution (500 mL) of sodium carbonate (Na2CO3) 2M and tetrakis (triphenylphosphine) palladium (0) [Pd (PPh3) 4] (7.7 g, 6.7 mmol) were added thereto and refluxed for 12 hours. After the reaction was completed, the mixture was cooled to room temperature, and the resulting mixture was extracted three times with water and toluene. The toluene layer was separated and dried with magnesium sulfate, and the filtrate was distilled under reduced pressure. The resulting mixture was recrystallized three times using chloroform and ethanol to obtain Compound P-1 (53.7 g, yield: 51%)

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; LG Chem, Ltd.; Jeong Min-u; Lee Dong-hun; Park Tae-yun; Cho Seong-mi; Moon Jeong-uk; Lee Jeong-ha; (34 pag.)KR2018/10149; (2018); A;,
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 20555-91-3 as follows. SDS of cas: 20555-91-3

Alternative Preparation of 2-(3,4-dichloro-phenylamino)-propionic Acid; A mixture of 3,4-dichloroiodobenzene (1.50 g, 5.50 mmol), L-alanine (734 mg, 8.25 mmol), copper(I) iodide, 2-hydroxybenzaldehyde phenylhydrazone (233 mg, 1.10 mmol), tri-potassium phosphate (3.50 g, 16.5 mmol), and N,N-dimethylformamide (8 mL) was stirred at 80 C. for 40 h, then after cooling diluted with water and acidified to pH 3 by addition of 37% aq. HCl solution. The mixture was extracted with EtOAc, the organic phase was washed with brine, dried (MgSO4), filtered, and evaporated. Chromatography (SiO2; EtOAc) afforded the title compound (1.08 g, 67%) as a 71:29 mixture of the (S) and (R) stereoisomers (accordingly, when D-alanine was used instead of L-alanine as starting material, the title compound was obtained as a 29:71 mixture of the (S) and (R) stereoisomers). Brown solid, MS: 232.1 (M-H)-.

According to the analysis of related databases, 20555-91-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Adam, Jean-Michel; Aebi, Johannes; Binggeli, Alfred; Green, Luke; Hartmann, Guido; Maerki, Hans P.; Mattei, Patrizio; Ricklin, Fabienne; Roche, Olivier; US2010/22518; (2010); 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. 202982-67-0, name is 4-Chloro-3-fluoroiodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 202982-67-0

A few drops of l -chloro-2-fluoro-4-iodobenzene (31.1 g, 121 mmol) in 50 mL of diethyl ether was added to the mixture of magnesium turnings (3.29 g, 136 mmol) and diethyl ether (50 mL) under nitrogen. After the reaction was initiated, the rest of the l-chloro-2-fluoro-4-iodobenzene ether solution was added at room temperature, and the reaction mixture was stirred at the same temperature for 1 h. This grignard reagent solution was added slowly to a solution of tert-butyl 4-(l-cyano-2- methoxy-2-oxoethy lidene)piperi dine- 1-carboxy late (10 g, 35.7 mmol) and copper(I) iodide (1.631 g, 8.56 mmol) in THF (200 mL) at 0 C, and the reaction mixture was stirred at 0 C for 1 h. Saturated ammonium chloride solution (100ml) was added, and the mixture was diluted with 500ml of ethyl acetate. The organic layer was washed with the water and brine solution, dried with the sodium sulphate and concentrated. The crude product was purified via silica gel chromatography eluteing with 20% of ethyl acetate in pet ether to give tert-butyl 4-(4-chloro-3-fluorophenyl)-4-(l-cyano-2-methoxy-2- oxoethyl)piperi dine- 1-carboxy late (12 g, 77%).

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; BRISTOL-MYERS SQUIBB COMPANY; WU, Yong-Jin; GUERNON, Jason M.; (102 pag.)WO2018/81384; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com