Author: Jessica.F

Adding a certain compound to certain chemical reactions, such as: 104539-21-1, name is 1-Iodo-2-(2-methoxyethoxy)ethane, 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 104539-21-1, name: 1-Iodo-2-(2-methoxyethoxy)ethane

STR27 100 mg (0.240 mmol) of Compound 5 synthesised in Reference Example 4 was dissolved in 1.0 ml of anhydrous DMF. To this solution, 166 mg (1.20 mmol) of potassium carbonate and a solution of 276 mg (1.20 mmol) of 1-iodo-2-(2-methoxyethoxy)ethane in 0.5 ml of anhydrous DMF were added. This reaction mixture was stirred at room temperature for 8 hours and 25 minutes. The reaction mixture was then added to a saturated aqueous solution of sodium chloride. The mixture was then extracted with ethyl acetate. The extract layer was washed with a saturated aqueous solution of sodium chloride two times, dried over magnesium sulfate, and concentrated. The residue was chromatographed on silica gel and eluted with a mixed solvent of ethyl acetate and hexane (1:1), whereby ethyl (E)-7-[4′-fluoro-5-[2-(2-methoxyethoxy)ethoxy]-3-(propan-2-yl)biphenyl-2-yl]-3,5-dihydroxy-6-heptenoate (Compound 11) was obtained in the form of a colorless oil in a yield of 26 mg (20.9%). 1 H-NMR (300 MHz, CDCl3) delta 1.18-1.33(m, 1H), 1.21(d, J=6.8 Hz, 3H), 1.22(d, J=6.8 Hz, 3H), 1.28(t, J=7.1 Hz, 3H), 1.38-1.53(m, 1H), 2.33-2.50(m, 2H), 2.84(d, J=2.0 Hz, 1H), 3.23(hept, J=6.8 Hz, 1H), 3.39(s, 3H), 3.52-3.64(m, 2H), 3.61(d, J=2.3 Hz, 1H), 3.68-3.76(m, 2H), 3.80-3.92(m, 2H), 4.02-4.22(m, 3H), 4.18(q, J=7.1 Hz, 2H), 4.22-4.40(m, 1H), 5.19(dd, J=16.0 and 6.4 Hz, 1H), 6.51(d, J=16.0 Hz, 1H), 6.65(d, J=2.7 Hz, 1H), 6.88(d, J=2.7 Hz, 1H), 6.96-7.06(m, 2H), 7.16-7.24 m, 2H)ppm. IR (liquid film): 3456, 2964, 2932, 1736, 1602, 1512cm-1. Mass (m/z, %): 518 (M+, 52), 500 (32), 454 (93), 369 (32), 267 (32), 241 (36), 239 (43), 230 (15), 183 (20), 103 (57), 59 (100).

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-Iodo-2-(2-methoxyethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Fujirebio Inc.; US5393780; (1995); A;,
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. 116632-39-4, name is 5-Bromo-2-iodotoluene, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Bromo-2-iodotoluene

4-Bromo-1 -iodo-2-methylbenzene, 5.00 g (16.8 mmol), and N-bromosuccinimide, 3.06 g (20.2 mmol), were dissolved into 50 mL of 1,2-dichloroethane. 2,2′-Azobisisobutyronitrile, 0.28 g (1.7 mmol), was added to the above solution at 85C and the resulting mixture was stirred at this temperature for 3 hours under nitrogen atmosphere. The solvent was removed in vacuo and the residue was purified by silica gel column chromatography to give 3.01 g (48%) of the product as a white solid. 1H-NMR (400 MHz, CDCI3): delta [ppm] = 4.54 (s, 2H), 7.13-7.16 (m, 1H), 7.63 (d, 1H), 7.73 (d, 1H).

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; BAYER PHARMA AKTIENGESELLSCHAFT; WORTMANN, Lars; SAUTIER, Brice; EIS, Knut; BRIEM, Hans; BOeHNKE, Niels; VON NUSSBAUM, Franz; HILLIG, Roman; BADER, Benjamin; SCHROeDER, Jens; PETERSEN, Kirstin; LIENAU, Philip; WENGNER, Antje, Margret; MOOSMAYER, Dieter; WANG, Qiuwen; SCHICK, Hans; (510 pag.)WO2018/172250; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 3032-81-3, 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 3032-81-3 as follows.

EXAMPLE 4; Step A. tert-Butyl 3-{[4-((2RS)-2-{[5-chloro-1-(3,5-dichlorophenyl)-1H-indol-2-yl]carbonyl}pentyl)benzoyl]amino}propanoate; To a vial containing the title compound of Example 3 Step D (100 mg, 0.26 mmol), were added 3,5-dichloro iodobenzene (0.045 mL, 0.31 mmol), copper iodide (2.5 mg, 0.012 mmol), potassium phosphate (116 mg, 0.55 mmol), and 1,2-trans-N,N-dimethylcyclohexane diamine (0.0082 mL, 0.05 mmol). The reaction mixture was placed under a nitrogen atmosphere, and anhydrous toluene (0.300 mL, deoxygenated via nitrogen sparge), was added. The vial was then capped and placed in a pre-heated oil bath (110¡ã C.) and stirred rapidly for 20 h. The mixture was allowed to cool to room temperature, then was filtered through a silica gel plug, eluting with EtOAc. The filtrate was concentrated in vacuo: LCMS B, tr=3.10 min, m/z 528.1 [M+H]+. The crude adduct was dissolved in 1,4-dioxane (1.5 mL). 2 N aq. LiOH (1.3 mL, 2.6 mmol) was added, and the resultant mixture was stirred at 50¡ã C. for 1 h. The mixture was allowed to cool to room temperature whereupon it was quenched by the addition of 2 N aq. HCl. The aqueous phase was extracted with EtOAc, and the organic phase was dried over Na2SO4 and concentrated in vacuo. To the crude carboxylic acid obtained above were added EDC (150 mg, 0.78 mmol), HOBt (105 mg, 0.78 mmol), and beta-alanine tert-butyl ester hydrochloride (141 mg, 0.78 mmol). The resultant mixture was dissolved in DMF (2 mL), DIEA (0.275 mL, 1.56 mmol) was added, and the reaction mixture was stirred at 50¡ã C. for 18 h. The reaction mixture was quenched by addition of sat. aq. NH4Cl, and the aqueous phase was extracted with EtOAc. The organic phase was concentrated in vacuo. Purification by flash chromatography on silica gel (0 to 70percent, then 70 to 100percent EtOAc in hexanes) provided the title compound: LCMS B, tr=3.01 min, m/z 663.1 [M+H]+; 1H NMR (500 MHz, CDCl3) delta 7.67 (d, J=2.0 Hz, 1H), 7.66 (s, 1H), 7.65 (d, J=8.0 Hz, 2H), 7.46 (t, J=7.0 Hz, 1H), 7.27-7.21 (m, 4H), 6.96 (d, J=8.0 Hz, 2H), 8.87 (t, J=5.5 Hz, 1H), 3.65 (q, J=6.0 Hz, 2H), 3.64-3.59 (m, 1 H), 3.04 (dd, J=14.0, 9.0 Hz, 1H), 2.83 (dd, J=14.0, 5.5 Hz, 1H), 2.52 (t, J=6.0 Hz, 1H), 1.80-1.73 (m, 1H), 1.59-1.52 (m, 1H), 1.44 (s, 9H), 1.41-1.33 (m, 2H), 0.92 (t, J=7.0 Hz, 3H).

According to the analysis of related databases, 3032-81-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Kim, Ronald M.; Bittner, Amy R.; Sinz, Christopher Joseph; Parmee, Emma R.; US2007/88071; (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. 33348-34-4, name is 4-Amino-3-iodobenzonitrile, A new synthetic method of this compound is introduced below., Product Details of 33348-34-4

To a solution of 4-amino-3-iodobenzonitrile in THF (4 ml.) was added BH3.THF (1 M solution in THF 2.5 ml.) drop-wise. The reaction mixture was refluxed for 3 h and 2 N HCI (1.0 ml.) was added . The resulting mixture was refluxed for an additional 1 h and then concentrated in vacuo in order to afford the crude, which was re-crystallized in MeOH for characterization to give 150 mg (74 %) of yellow powder. 4-amino-3-iodobenzylammonium chloride. ^ NMR (250 MHz, DMF) d 8.90 (s, broad, 3H, +NH3), 7.88 (d, J = 2.0 Hz, 1H, CHar), 7.42 (dd, J = 8.3, 2.1 Hz, 1H, CHar), 6.93 (d, J = 8.3 Hz, 1H, CHar), 5.81 (s, 6H, HCI), 4.06 (q, J = 5.6 Hz, 2H, CH2). (0104) 13C NMR (63 MHz, DMF) d 151.64 (Car-+NH3), 149.11(Car), 140.44 (CHar), 131.17 (CHar), 124.75 (Car), 114.86 (CHar), 82.93(Car-I), 42.30 (CH2).

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; UNIVERSIDAD COMPLUTENSE DE MADRID; FUNDACION PARA LA INVESTIGACION BIOMEDICA DEL HOSPITAL INFANTIL UNIVERSITARIO NINO JESUS; FUNDACION PARA LA INVESTIGACION BIOMEDICA DEL HOSPITAL UNIVERSITARIO LA PRINCESA; VALLET REGI, Maria; BAEZA GARCIA, Alejandro; VILLAVERDE CANTIZANO, Gonzalo; CASTILLO ROMERO, Rafael; RAMIREZ ORELLANA, Manuel; MELEN FRAJLICH, Gustavo; GONZALEZ MURILLO, Africa; ALFRANCA GONZALEZ, Arantzazu; (49 pag.)WO2019/185586; (2019); 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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 181765-86-6

In a 500-mL round-bottom flask reactor, methyl 5-bromo-2-iodobenzoate (25.0 g, 73 mmol), 4-dibenzofuran boronic acid (18.7 g, 88 mmol), tetrakis (triphenylphosphine)palladium (1.7 g, 0.15 mmol), and potassium carbonate (20.2 g, 146.7 mmol) stirred together with toluene (125 mL), tetrahydrofuran (125 mL), and water (50 mL) for 10 hrs at 80 C. After completion of the reaction, the reaction mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer thus formed was separated, concentrated in a vacuum, and purified by column chromatography to afford . (75.0 g, 60.1%).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC CO., LTD.; Pyo, Sung-Wan; Shim, So Young; Lee, Yun-Ah; Yu, Se Jin; (119 pag.)US2017/141321; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 77317-55-6, 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. 77317-55-6, name is Methyl 2-amino-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under an argon atmosphere 200 mg (0.72 mmol) 2-amino-5-iodo-benzoic acid methyl ester is dissolved in 4.0 ml toluene, 156 mg (0.94 mmol) 2-ethoxy-phenylboronic acid, a solution of 475 mg (2.17 mmol) tripotassium phosphate in 0.5 ml water, 53 mg (0.06 mmol) Pd2(dba)3, and 28 mg (0.10 mmol) N-phenyl-2-di-tert.-butylphosphinopyrrole are added. The reaction mixture is heated to 100 C. and stirred over night. After cooling to room temperature the reaction mixture is filterd over celite and the filtrate is evaporated under reduced pressure. The residue is purified by preparative HPLC (eluent A: water+0.13% TFA, eluent B: acetonitrile). The product is dissolved in dichloromethane and extracted with a saturated aqueous solution of Na2CO3. The organic layer is dried and evaporated under reduced pressure. yield: 40 mgRT (Microsorb 1s)=1.72 minESI-MS (M-FH)+=272

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-amino-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2010/249158; (2010); A1;,
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 61272-76-2 as follows. name: 4-Fluoro-2-iodoaniline

General procedure: A 25 mL Wattecs reaction tube was charged with 2-haloaniline 1 (0.6 mmol), potassium O-ethyl dithiocarbonate 2 (1.8 mmol),CuCl (0.06 mmol), and DMF (2 mL). The reaction vessel was flushed with argon three times and sealed. Then the mixture was stirred electromagnetically in an oil bath at 110¡ãC for 6 h.The reaction process was monitored by TLC on silica gel. After the reaction was completed, the reaction mixture was cooled to room temperature, and then HCl (3 mL, 3 mol/L) was added and stirred for another 30 min. The reaction mixture solution was extracted by ethyl acetate (3 ¡Á 20 mL). Subsequently, the combined organic solutions were dried by anhydrous sodium sulfate and the target product was purified by chromatography on a silica gel column (eluent: petroleum ether/ethyl acetate) togive the corresponding pure product 3. Complete characterization characterizationof the products (all known) is found in the Supplemental Materials (Figures S1?S13).

According to the analysis of related databases, 61272-76-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Lei; Zhu, Ning; Gao, Min; Zhao, Xiaole; Han, Limin; Hong, Hailong; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 191; 5; (2016); p. 699 – 701;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 83863-33-6, These common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, 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.

9.97 g of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide (30.3 mmol) and 5.03 g of potassium iodide (30.3 mmol) in 75 ml. of cyclohexanol were stirred for 1 h at 800C. After addition of 7.7 g of sodium carbonate (72.7 mmol) and 5.65 g of 5-iodo-2-methyl- aniline (24.2 mmol), stirring continued for deltah at 1600C. At room temperature, the mixture was filtered, washed with dichloromethane, and the filtrate evaporated to dryness. The residue was dissolved in dichloromethane, filtered, and the solvent evaporated. The remaining residue was trituated with n-heptane and the crystalline product filtered off, washed several times with n-heptane and dried in vacuo to yield 10.7 g of product

The synthetic route of 83863-33-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT GMBH &; CO. KG; ABBOTT LABORATORIES; HAUPT, Andreas; POHLKI, Frauke; DRESCHER, Karla; WICKE, Karsten; UNGER, Liliane; RELO, Ana-Lucia; BESPALOV, Anton; VOGG, Barbara; BACKFISCH, Gisela; DELZER, Juergen; ZHANG, Min; LAO, Yanbin; WO2010/125134; (2010); 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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C6H5ClIN

A solution of 3-CHLORO-4-IODO-ANILINE (5. 6G), ISOAMYLNITRITE (8. 8ML) and ETHYLDISULPHIDE (13. 4ML) in acetonitrile (100ml) was heated at 60C for 24h. The solvent was removed under reduced pressure and the residue purified by chromatography on silica eluting with 1% ETHYLACETATE/ISOHEXANE. YIELD 4. 02G ‘H NMR CDC13 : 8 7. 70 (1H, D) ; 7. 36 (1H, d); 6. 87 (1H, dd); 2. 94 (2H, q) ; 1. 32 (3H, t)

The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 3032-81-3, A common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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 suspension of DL-5-methoxypyrrolidin-2-one (3a) or arylaminopyrrolidinones 3b,c (1 equiv), CuI (0.5 equiv), cesium carbonate (2 equiv), and corresponding aryl iodide (1 equiv) in dioxane was placed under a nitrogen atmosphere. The coupling ligand DMEDA (1 equiv) was added dropwise by using a syringe and the mixture was then stirred at 60 ¡ãC for various periods of time (14?88 h). At the end ofthe reaction, the insoluble salts deposited after cooling at r.t. were collected by filtration then washed with dichloromethane. The resulting filtrate was concentrated in vacuo and the residue was partitioned between water and dichloromethane. The organic layer was dried on MgSO4 and evaporated to dryness. The residue was finally purified by chromatography on silica gel column (EtOAc/n-heptane) to afford pure N-arylated compound 40?44.

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Baudelet, Davy; Daich, Adam; Rigo, Benoit; Lipka, Emmanuelle; Gautret, Philippe; Homerin, Germain; Claverie, Christelle; Rousseau, Jolanta; Abuhaie, Cristina-Maria; Ghinet, Alina; Synthesis; vol. 48; 14; (2016); p. 2226 – 2244;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com