Tag: M.W=200-300

Related Products of 25309-64-2, These common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-iodobenzene, 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.

In a typical experiment, known quantities of iodobenzene (1.0 mmol), phenylacetylene (1.2 mmol), P(DVB-IL)-Pd (20 mg, Pd 0.5 mol %), Et3N (0.4 mL, 2.4 mmol), and distilled water (5.0 mL) were charged into the reactor. The autoclave was closed, purged three times with CO, pressurized to 3.0 MPa with CO, and then stirred at 130 C for 6 h. After cooling down to room temperature, the reaction mixture was analyzed by GC-MS and then worked up by removing water under vacuum and the residue was purified by chromatography on silica gel (eluting solvent hexane:ethyl acetate).

The synthetic route of 25309-64-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Yan; Liu, Jianhua; Xia, Chungu; Tetrahedron Letters; vol. 52; 14; (2011); p. 1587 – 1591;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 29289-13-2, A common heterocyclic compound, 29289-13-2, name is 2-Iodo-4-methylaniline, molecular formula is C7H8IN, 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 solution of 2-iodoaniline (333.6 mg, 1.52 mmol, 1.0 equiv) in DCM (5.0 mL) was added with Et3N (0.23 mL, 166.9 mg, 1.65 mmol, 1.1 equiv). The reaction solution was cooled at 0 C and acetyl chloride (0.28 mL, 308 mg, 3.92 mmol, 2.6 equiv) was added into the cooled solution. The resulting mixture was warmed to stir at room temperature overnight. Upon completion, thereaction was added with water and the separated aqueous phase was extracted with EtOAc (3xtimes). The combined organic phases were washed with sat. aq. NaCl, dried over anh. Na2SO4 and concentrated under reduced pressure. The crude material was purified by SiO2 column chromatography eluting with 30% EtOAc-hexane to yield 387.9 mg (98%) of the corresponding N-(2-iodophenyl)acetamide as a white solid.

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; Chaisan, Nattawadee; Kaewsri, Wilailak; Thongsornkleeb, Charnsak; Tummatorn, Jumreang; Ruchirawat, Somsak; Tetrahedron Letters; (2018); p. 675 – 680;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 181765-85-5, 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. 181765-85-5, name is Methyl 4-chloro-2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Arene (0.10 mmol, 1.0 equiv), Pd(OAc)2 (2.2 mg, 10 mumol,10 mol%), ligand (15 mol% or 20 mol%), hydrogen phosphate (15 mol% for benzylamine substrate), aryl iodide (0.3 mmol, 3.0 equiv.) and silver acetate (50 mg, 0.30 mmol, 3.0 equiv.) were added into a 2-dram reaction vial. Solvent and (+)-NBE-CO2Me (20 mol% or 50 mol%) were added to the mixture. The vial was flushed with N2 and capped. The reaction mixture was then stirred at the selected temperature for 12-24 h. After cooling to room temperature, the mixture was filtered through Celite and eluted with ethyl acetate. The filtrate was evaporated under reduced pressure. Purification by preparative thin-layer chromatography afforded the desired product.

The chemical industry reduces the impact on the environment during synthesis Methyl 4-chloro-2-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Article; Shi, Hang; Herron, Alastair N.; Shao, Ying; Shao, Qian; Yu, Jin-Quan; Nature; vol. 558; 7711; (2018); p. 581 – 585;,
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. 27913-58-2, name is 4-(4-Iodophenyl)butanoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C10H11IO2

[0240] A flask was charged with 4-(p-iodophenyl)butyric acid (600 mg, 2.07 mmol), DCC (427 mg, 2.07 mmol), and N-hydroxysuccinimide (238 mg, 2.07 mmol). Diehl or omethane (6 mL) was added, and the reaction stirred at room temperature for 4 h. Filtering the reaction mixture through a short celite pad, rinsing the pad with dichl or omethane (5 mL), and removing the solvent under vacuum provided crude 4- (p-iodophenyl)butyric acid NHS ester. To this was added DMF (8 mL), 4- aminobutyric acid (525 mg, 5.19 mmol), and diisopropylethylamine (2 mL). The reaction was stirred at room temperature for 24 h, then loaded onto a 100 g Cl 8 Isco gold column. Eluting with 15% to 85% acetonitrile in water with 0.1% TFA provided 70 (560 mg, 1.49 mmol, 72% yield).

The synthetic route of 27913-58-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TARVEDA THERAPEUTICS, INC.; BILODEAU, Mark T.; MOREAU, Benoit; KADIYALA, Sudhakar; WOOSTER, Richard; WHITE, Brian H.; (102 pag.)WO2019/195384; (2019); 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. 35944-64-0, name is 3-Iodo-4-methylaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 3-Iodo-4-methylaniline

1.2.1.2. Illustrative synthesis of Intermediate Gen-3-a: 4-Methyl-3-(4,4,5,5-tetramethyl- [l,3,2]dioxaborolan-2- l)-phenylamine To a suspension, previously degazed with nitrogen bubbling for 1 h, of Intermediate Gen-2-b (300 g, 1.29 mol, 1 eq.), Intermediate Gen-9-a (343.2 g, 1.35 mol, 1.05 eq.) and potassium acetate (380 g, 3.9 mol, 3 eq.) in DMSO (2.65 L), previously degazed with nitrogen bubbling for 2 h, is added PdCl2(dppf).DCM (52 g, 0.06 mol, 0.05 eq.). The reaction mixture is stirred at 80C under nitrogen overnight. The reaction is cooled to room temperature, then water (1.5 L) and EtOAc (3 L) are added. The biphasic solution is filtered through a plug of celite, and the cake is washed with EtOAc (2 L). The two layers of the filtrate are separated, the aqueous layer is extracted again with EtOAc (3 L) and the combined organic layers are washed with water (500 mL). The organic layer is dried over Na2SO i, filtered and evaporated to dryness. The residue is purified by chromatography on silica (elution cyclohexane/EtOAc: 95/5 to 70/30) to afford Intermediate Gen-3-a. lH NMR (300 MHz, CDCl3-i ) delta ppm 7.17 (1 H, d), 6.99 (1 H, d), 6.70 (1 H, dd), 3.54 (2 H, bs), 2.25 (3 H, s), 1.36 (12 H, s)

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; GALAPAGOS NV; SANIERE, Laurent Raymond Maurice; HUCK, Jacques; DYKES, Graeme James; SCHMITT, Benoit Antoine; BLANC, Javier; BUTLER, Anna Sara; BEAUMONT, Stephane Nicolas Alain; BONNATERRE, Florence Marie-Emilie; WO2015/24905; (2015); 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. 3718-88-5, name is 3-Iodobenzylamine hydrochloride, A new synthetic method of this compound is introduced below., Recommanded Product: 3718-88-5

Resin 1 (obtained from previous synthesis) (100 mg, 0.077 mmol) was swelled in DCM (2 mL) for 1 h anddrained. A solution of 3-iodobenzylamane hydrochloride 2 (83.0 mg, 0.308 mmol) and Et3N (250 mL, 1.80 mmol) in DMF(1.5 mL) was purged with a stream of N2 bubbles for two minutes and added to the resin. After mixing for 5 min,PdCl2(PPh3)2 (11.0 mg, 0.016 mmol) and CuI (7.0 mg, 0.037 mmol) were added and the mixture shaken for 36 h. Theresin was drained, washed with DMF (4 3 2 mL), DCM (4 3 2 mL) and cleaved with 10% TFA/DCM (1.5 mL) for 20min. The solution was collected and the resin was rinsed with additional 10% TFA/DCM (1.5 mL). The cleavage fractionswere combined, treated with neat TFA (3.0 mL), stirred for 1 h at rt and concentrated by rotary evaporation to give acrude brown residue. Purification by RP-HPLC (C18 column, CH3CN gradient 5-65%, 0.1% TFA, UV analysis 300 nm,28 min) and lyophilization of the collected fractions afforded 4.3 mg (14%) of (2S,3R)-4-[4-(3-aminomethyl-phenyl)-buta-1,3-diynyl]-N-(2-hydroxy-1-hydroxycarbamoyl-propyl)-benzamide as a white solid. LRMS (ES+) m/z 392.0 (C22H21N3O4+ H requires 392.15); RP-HPLC (300 nm, 28 min run) 10.0 min.

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 University of Washington; Novartis Vaccines and Diagnostics, Inc.; Andersen, Niels H.; Bowman, Jason; Erwin, Alice; Harwood, Eric; Kline, Toni; Mdluli, Khisimuzi; Ng, Simon; Pfister, Keith B.; Shawar, Ribhi; Wagman, Allan; Yabannavar, Asha; EP2295402; (2015); 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. 144550-76-5, name is Methyl 2-amino-4-iodobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 144550-76-5

13.8 g of methyl 2-amino-4-iodobenzoate are treated with 48 ml of glacial acetic acid and subsequently with 86 ml of concentrated hydrochloric acid. A solution of 3.8 g of sodium nitrite in 15 ml of water is slowly added dropwise to this suspension which is cooled to -5 C., and stirring is continued at this temperature for 30 minutes. This cooled diazonium salt solution is added dropwise at 0 C. to a solution of 20 ml of sulfur dioxide, 60 ml of glacial acetic acid, 10 ml of water and 3.1 g of copper(II) chloride dihydrate, and stirring is continued first for 1 hour at 0 C. and then overnight at room temperature. The reaction mixture is poured into 1 l of ice-water, and the product is filtered off with suction. This gives 12.7 g of bis(2-methoxycarbonyl-5-iodobenzene)disulfide of m.p. 133 C.-135 C.

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; ROTAM AGROCHEM INTERNATIONAL COMPANY LIMITED; BRISTOW, James Timothy; (11 pag.)US2017/121294; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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 627-31-6, Formula: C3H6I2

General procedure: A suspension of alkenyl- or aryl-dithiol(1.0 mmol), triethylamine (2.0 mmol), LR (0.44g, 1.0 mmol) or FcLR (0.56 g, 1.0 mmol) and dihaloalkane(1.0 mmol) in dry THF (60 mL) was stirred under N2 gas atmosphere at ambient temperature for 24 h leadingto a reddish yellow or pale-yellow suspension. Upon filtering to remove insoluble solid the filtrate was driedunder reduced pressure. The residue was dissolved in dichloromethane (ca. 2 mL) and was loaded onto a silicagel column (dichloromethane as eluent) to give the macrocycles. Another unexpected nine-membered ring 4was also obtained in respective 25% and 30% yields in the cases of 5 and 9. Two diastereomers wereseparated completely in the cases of 10 and 12.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

Reference:
Article; Hua, Guoxiong; Cordes, David B.; Slawin, Alexandra M. Z.; Woollins, J. Derek; Synlett; vol. 29; 11; (2018); p. 1496 – 1501;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 14452-30-3,Some common heterocyclic compound, 14452-30-3, name is 1-(3-Iodophenyl)ethanone, molecular formula is C8H7IO, 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-(3-iodophenyl)propan-2-ol; To a solution of 3-iodo-acetophenone (15g, 61 mmol) in 10OmL THF at -78 0C was slowly added MeMgBr (6OmL of a 1.4M solution in THF, 84 mmol) and the solution was stirred for 1 hour as it warmed to 0 0C. The reaction was quenched with saturated NH4Cl and the crude product was extracted with ether (2x) and the organic phases were dried over Na2SO4, filtered and concentrated in vacuo. The crude was purified by flash (5-10% EA/hex) to give the desired product.

The synthetic route of 14452-30-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK FROSST CANADA LTD.; WO2007/14454; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 401-81-0, A common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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.

Step C: Preparation of 1 ,3-dimethyl 2-[3-(trifluoromethyl)phenyl]propanedioateDioxane (100 mL) was purged with nitrogen gas for 10 minutes. Phenanthrolene (1.0 g) and copper (I) iodide (1.0 g) were added to the dioxane, the suspension was allowed to stir under a nitrogen atmosphere for 5 minutes, and then cesium carbonate (18.72 g, 57.45 mmol), dimethyl malonate (5.46 g, 50.6 mmol), and l-iodo-3-(trifluoromethyl)benzene (12.5 g, 46.0 mmol) were added. The reaction mixture was heated to reflux for 18 hours and then cooled to room temperature. Aqueous 1 N HC1 was added to the reaction mixture, the layers were separated, and the aqueous layer was extracted with ethyl acetate (3 x 100 mL). The combined organic layers were dried over magnesium sulfate and filtered. Celite diatomaceous filter aid (5 g) was added to the filtrate, and the resulting suspension was concentrated under reduced pressure at 50 C to yield a solid consisting of the crude product adsorbed onto Celite. This solid was purified by silica gel chromatography eluting with a gradient of 100% hexanes to 25% ethyl acetate in hexanes to yield 7.36 g (58.0%) of the title product. .H NMR (CDC13) delta 7.59-7.65 (m, 3H), 7.49 (t, 1H), 4.70 (s, 1H), 3.76 (s, 6H).

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; PAHUTSKI, Thomas, Francis., Jr.; WO2012/92115; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com