Month: July 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. 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. 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

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

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

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 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

Related Products of 610-97-9,Some common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, 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.

To a stirred solution of methyl 2-iodobenzoate (5.0 g, 19.08 mmol, 1 equiv) and NBS (3.73 g, 20.99 mmol, 1 .1 equiv) in acetic acid (10 mL) was added H2S04 (10 mL) drop wise at 20-40C. The reaction mixture was stirred for 88 h at room temperature and then heated to 50C & stirred for 4 h. The reaction mixture was cooled to 10C and quenched with cold water (40 mL) and extracted with DCM (3 x 50 mL). The organic layer was washed with 5% sodium bicarbonate (2 x 50 mL), 10% Na2S03 solution (50 mL), and water (50 mL), and then dried over sodium sulphate, and evaporated to obtain methyl 5-bromo-2- iodobenzoate as crude product which was purified over silica gel flash column chromatography. The compound eluted out in 10 % ethyl acetate in hexanes. The pure fractions were evaporated to obtain methyl 5-bromo-2-iodobenzoate as off white solid (5 g, 77%). NMR (400 MHz, CDCI3) delta ppm 3.94 (s, 3 H).7.26 – 7.29 (m, 1 H), 7.83 (d, J=8.4 Hz, 1 H), 7.93 (d, J=8.8 Hz, 1 H).

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

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; AXTEN, Jeffrey; KETHIRI, Raghava Reddy; KRISTAM, Rajendra; VENKATESHAPPA, Chandregowda; (162 pag.)WO2018/15879; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

77317-55-6, name is Methyl 2-amino-5-iodobenzoate, 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. Recommanded Product: Methyl 2-amino-5-iodobenzoate

Methyl anthranilate (15) (2.0 g, 13.2 mmol), granulatediodine (3.36 g, 13.2 mmol) and hydrogen peroxide-urea(1.24 g, 13.2 mmol), were dissolved in 20 mL of ethylacetate. The reaction mixture was stirred for 1.5 h at roomtemperature and then washed with sodium thiosulfate(3 × 10 mL) and water (3 × 10 mL); then solvent wasevaporated under reduced pressure to afford methyl2-amino-5-iodobenzoate (16) as a brown solid (3.33 g,yield 91%). The solid was hydrolyzed using NaOH/MeOH(5%) to give 2-amino-5-iodobenzoic acid (17) (2.81 g, yield89%). Finally, the acid was cyclized with triphosgene andtriethylamine as base affording 6-iodoisatoic anhydride(6-iodo-1H-benzo[d][1,3]oxazine-2,4-dione, 2) with a76% yield (2.34 g).

The synthetic route of 77317-55-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; De La Cruz, Armando; Vega-Acevedo, Carlos Alejandro; Rivero, Ignacio A.; Chavez, Daniel; Journal of the Brazilian Chemical Society; vol. 29; 8; (2018); p. 1607 – 1611;,
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. 74-88-4, name is Iodomethane, A new synthetic method of this compound is introduced below., SDS of cas: 74-88-4

m-Iodophenol (5.5 g, 25 mmol) was dissolved in water containing KOH (1.4 g, 25 mmol). A cold solution of diazotized sulfanilic acid (5.1 g, 27.5 mmol) was added to the mixture with stirring at rt for 30 min followed by the addition of sodium hydrosulfite (12 g, 69 mmol). The colour of the solution was changed immediately upon the addition of sodium hydrosulfite and the solution was stirred at 45 C for 20 min. Diethyl ether was added to the mixture, the mixture was filtered and the filtrate was concentrated. The solid was recrystallized from hot water to yield needles. Methyl iodide was added (0.98 mL, 15.7 mmol) to 4-amino-3-iodophenol (3.71 g, 15.8 mmol) in DMF (70 mL) in the presence of Cs2CO3 (13.45 g, 41.3 mmol). The reaction was left at rt for 48 h. The mixture was then diluted with water, extracted with diethyl ether, the combined organic extracts were washed with water, dried over Na2SO4, filtered and concentrated. The product was purified by silica gel column chromatography (PE/EtOAc 9:1) and obtained 4-methoxy-2-iodoaniline (15) as a light brown oil (3.36 g, 54%) from m-iodophenol.To a solution of 4-methoxy-2-iodoaniline (3.0 g, 12.0 mmol) in THF (20 mL) was added di-tert-butyl dicarbonate (3.15 g, 14.5 mmol). The reaction mixture was refluxed for 2 days then quenched with water (15 mL). The solution was extracted with Et2O (3×20 mL) and the combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated. The crude mixture was purified by silica gel column chromatography (2% EtOAc in PE) to yield N-Boc-2-iodo-4-methoxy aniline as a light brown solid (3.72 g, 89%). 1H NMR (500 MHz, CDCl3, delta): 7.82 (s, 1H), 7.29 (d, J=3.0 Hz, 1H), 6.88 (dd, J=9.0, 3.0 Hz, 1H), 6.53 (s, 1H), 3.75 (s, 3H), 1.52 (s, 9H); 13C NMR (125 MHz, CDCl3, delta): 156.21, 153.21, 132.54, 123.89, 122.24, 115.05, 80.87, 55.85, 28.48; IR (KBr, cm-1): 3322, 2983, 1718; HRMS (ESI): (M+Na)+ calcd for +C12H163INNaO 372.0067, found 372.0071.

The synthetic route of 74-88-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Jana, Goutam Kumar; Sinha, Surajit; Tetrahedron; vol. 68; 35; (2012); p. 7155 – 7165;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 6937-34-4, 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. 6937-34-4, name is 3-Iodophthalic acid, This compound has unique chemical properties. The synthetic route is as follows.

A solution of 3-iodophthalic acid (0.9 g, 3.08 mmol) in acetic anhydride (5 mL) was heated to reflux under nitrogen overnight. After cooling, the solvent was removed in vacuo and the residue purified by trituration with ethanol to give 4-iodo-2-benzofuran-1,3-dione (0.55 g, 65%).

The chemical industry reduces the impact on the environment during synthesis 3-Iodophthalic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK SHARP & DOHME LIMITED; WO2006/21805; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com