Tag: M.W=300-400

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Computed Properties of C5H10I2

Synthesis of Compound 59.1 [0424] To a solution of tert-butyl 2-(hydroxymethyl)pyrrolidine-l -carboxylate (1.0 g, 4.9 mmol, 1.0 eq) in MeCN (50 mL) were added NaOH (0.39 g, 9.8 mmol, 2.0 eq) and 1, 5- diiodopentane (3.2 g, 9.9 mmol, 2.0 eq). The reaction mixture was stirred at room temperature for 48 h and concentrated under reduced pressure. The residue was diluted with ethyl acetate (100 mL), washed with H20 (100 mL) and brine (50 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column (PE : EA = 5 : 1) to give 59.1 (0.7 g, Y: 36%) as a yellow oil. 1H NMR (400 MHz, CDC13) delta: 3.96-3.92 (m, 1H), 3.54-3.51 (m, 1H), 3.48-3.39 (m, 2H), 3.33-3.32 (m, 3H), 3.19 (t, J = 6.8 Hz, 2H), 2.31-2.19 (m, 1H), 1.95-1.76 (m, 6H), 1.60-1.50 (m, 3H), 1.46 (s, 9H).

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, 1,5-Diiodopentane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BIOGEN IDEC MA INC.; JENKINS, Tracy; VESSELS, Jeffery; WO2014/143672; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 450412-29-0, These common heterocyclic compound, 450412-29-0, name is 1-Bromo-3-fluoro-2-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.

Step 2. 6-Bromo-2-fluoro-3′-methylbiphenyl: Pd(Ph3P)4 in a 500-mL round- bottom flask under N2 atmosphere was treated sequentially with a solution of 1- bromo-3-fluoro-2-iodo-benzene (30 g, 0.1 mol) in toluene (250 mL), a solution of 2N aq Na2CO3 (200 mL) and 3-methyl phenylboronic acid in ethanol (62 mL). This mixture was heated at reflux under N2 for 12 h, then cooled to rt. The mixture was partitioned between water and EtOAc. The combined organic layers were washed with brine, dried over MgSO4, evaporated and purified by column chromatography to give 6-bromo-2-fluoro-3′-methyl-biphenyl (12 g). 1H NMR (400MHz, CD3OD): 7.03 (m, 2H), 7.48-7.04 (m, 4H), 7.50 (d, IH).

The synthetic route of 450412-29-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; VITAE PHARMACEUTICALS, INC.; WO2008/124582; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, molecular formula is C8H6BrIO, 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. category: iodides-buliding-blocks

General procedure: Thiosemicarbazone 3 (0.317 g, 1.0 mmoles) was added to astirred solution of 2-bromo-1-(4-fluorophenyl)ethanone(0.217 g, 1.0 mmole) in DMF/EtOH (3: 2) (50 ml). Thereaction mixture was stirred under room temperature for 2 h,and separate precipitate was collected by filtration, suspendedin water and neutralized with NaHCO3 solution.The crude product was purified on silica gel column chromatography(230-400 mesh) using (dichloromethane/methanol, 80:20, Rf = 0.74) to afford the desired product:0.38 g, 87%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 31827-94-8, its application will become more common.

Reference:
Article; ??czkowski, Krzysztof Z.; Anusiak, Joanna; ?witalska, Marta; Dzitko, Katarzyna; Cytarska, Joanna; Baranowska-??czkowska, Angelika; Plech, Tomasz; Paneth, Agata; Wietrzyk, Joanna; Bia?czyk, Joanna; Medicinal Chemistry Research; vol. 27; 4; (2018); p. 1131 – 1148;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 31827-94-8, 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Carbothioamide 2 (0.396 g, 2.0 mmol) was added to a stirredsolution of 2-bromo-1-(4-fluorophenyl)ethanone (0.434g, 2.0 mmol) in absolute ethyl alcohol (25 ml). The reactionmixture was stirred at room temperature for 20 h. Next, thereaction mixture was added to water (50 ml) and neutralizedwith NaHCO3 solution. The product was extracted withdichloromethane (2 × 50 ml), the solvent was evaporated invacuo, and the solid was washed with diethyl ether to affordthe desired product to yield 0.27 g (43%)

The synthetic route of 2-Bromo-1-(4-iodophenyl)ethanone has been constantly updated, and we look forward to future research findings.

Reference:
Article; ??czkowski, Krzysztof Z.; Landowska, Katarzyna; Biernasiuk, Anna; Sa?at, Kinga; Furga?a, Anna; Plech, Tomasz; Malm, Anna; Medicinal Chemistry Research; vol. 26; 9; (2017); p. 2088 – 2104;,
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. 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 25252-00-0

Step I: To a stirred solution of 2-bromo-5-iodobenzoic acid (150 g, 458 mmol) in dichloromethane (1500 ml) was added DMF (2.0 ml) followed by oxalylchloride (58.2 ml, 688 mmol) at 0 C in drop wise fashion over the period of 30 min. After complete addition, the reaction mixture was stirred at room temperature for 3h. Volatiles were evaporated under reduced pressure to give 2-bromo-5-iodo-benzoyl chloride (-158 g). The crude product was used for the next step immediately. (Note: The product should not be exposed to air).

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NOVARTIS AG; BEBERNITZ, Gregory Raymond; BOCK, Mark Gary; WO2012/140596; (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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

General procedure: Sulfuric acid (400?800 muL) was added to a stirred mixture of iodoarene (1 mmol), Oxone (1 mmol, 617 mg) and arene (1.1?3 mmol) in acetonitrile (2 mL). The reaction mixture was stirred overnight and a solution of KBr (2 mmol, 240 mg) in water (10 mL) was added. After the formation of a solid or oily residue, acetonitrile was removed under reduced pressure. To the residue Et2O (10 mL) was added and the suspension stirred for 10 min. The precipitated diaryliodonium bromide was filtrated and washed with water (15 mL) and Et2O (15 mL). The product was dried under vacuo.

The synthetic route of 328-73-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Soldatova, Natalia; Postnikov, Pavel; Kukurina, Olga; Zhdankin, Viktor V.; Yoshimura, Akira; Wirth, Thomas; Yusubov, Mekhman S.; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 849 – 855;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, 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. Safety of 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

Example 3: Preparation of 3-{3-[(3,4-dimethoxy-bicyclo[4.2.0]octa-l,3,5-trien-7- ylmethyl)-methyl-amino]-propyl}-7,8-dimethoxy-l,3-dihydro-benzo[d]azepin-2- one (Formula-6) 7,8-Dimethoxy-3-(3-iodopropyl)- 1 ,3-dihydro-2H-3-benzazepin-2-one (Formula-4) (17.8g, 0.0456mol.) is added with (lS)-4,5-Dimethoxy-l-[(methylamino)methyl] benzocyclobutane hydrochloride (Formula-5) (9.29g, 0.0381mol.) in about 107ml. Acetone. To the mass, Potassium carbonate (12.7g, 0.0919mol.) is added and stirred for about 3hr. at 55 – 58C. The mass is filtered through celite bed at 35 – 40C. Filtrate is concentrated under reduced pressure at 45 – 50C to 1.4w/w. To the residual mass, 89ml of ethyl acetate is added and the product is extracted using 3N HC1 solution thrice (89ml, 2 x 35.6ml). The combined aqueous layer is basified using Sodium hydroxide and extracted the product using ethyl acetate thrice (89ml. 2 x 36.5ml). The combined organic layer is washed with water and then concentrated under vacuum at 45 – 50C to obtain about 19.29g (85%) of 3-{3-[(3,4-dimethoxy-bicyclo[4.2.0]octa-l,3,5-trien-7-ylmethyl)- methyl-amino]-propyl}-7,8-dimethoxy-l,3-dihydro-benzo[d]azepin-2-one (Formula-6) having the purity >75%>

The synthetic route of 148870-57-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOCON LIMITED; KOTHAKONDA, Kiran Kumar; RAMASAMY, Sivakumar; BANDARU, Sravan Kumar; VENKATA, Srinivas Pullela; WO2014/20534; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 181765-86-6, 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. 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.

In an argon atmosphere, 31 methyl 5-bromo-2-iodobenzoate (2.50 g, 7.33 mmol) and 32 tetrakis(triphenylphosphine)palladium (423 mg, 5 mol %) were dissolved in 30 mL of 33 tetrahydrofuran (THF). At ambient temperature 34 2-thienylzinc bromide (1.67 g, 7.33 mmol) was added dropwise, the solution was vigorously stirred and heated to 70 C. overnight. The reaction was stopped with a 2M solution of 35 HCl and the organic phase extracted with diethylether, washed with water and brine, dried over sodium sulfate (Na2SO4), filtered and concentrated in vacuo. The crude product was purified by silica gel chromatography eluting with n-hexane/dichloromethane (DCM): 9:1 (v/v) then 7:3 (v/v), whereby a colourless 36 oil was obtained (2.15 g, 7.24 mmol, 98.7%). (0105) 1H NMR (CDCl3, 200 MHz): delta=7.86 (dd, 1H, 1=4.8 Hz, 1=0.3 Hz, Har), 7.61 (dd, 1H, J=2.1 Hz, 1=8.3 Hz, Har), 7.35 (m, 2H, Har), 7.04 (m, 2H, Har), 3.75 (s, 3H). (0106) 13C NMR (CDCl3, 50 MHz): delta=167.3; 141.1; 134.2; 134.1; 133.3; 133.0; 132.5; 127.7; 127.1; 136.6; 121.9; 62.1; 14.3.

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 5-bromo-2-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; COMMISSARIAT A L’ENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES; Demadrille, Renaud; Kervella, Yann; Joly, Damien; Godfroy, Maxime; US2019/144677; (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. 702641-04-1, name is 2-Iodo-5-(trifluoromethyl)benzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 702641-04-1

F. Isopropyl 5-TRIFLUOROMETHYL-2-IODOPHENYLACETATE A mixture OF 4-AMINOBENZOTRIFLUORIDE (100 g, 0.62 mol) and di-tert-butyl carbonate (150 G, 0.69 mol) in anhydrous THF (400 mL) is heated at reflux temperature for 6 hours and then cooled to room temperature. Most of the solvent is removed using a rotary evaporator and the non-volatile material that remains is triturated with water (1000 mL) to form a solid. The solid is isolated by filtration and washed with additional water (500 mL), then washed with hexanes (500 mL) to give 4- (BOC-amino) benzotrifluoride (m. p. 123-124C). 4- (BOC-AMINO) BENZOTRIFLUORIDE (143 g, 0.55 mol) is dissolved in anhydrous THF (800 mL) and cooled in a dry-ice/ethanol bath. A solution of TERT-BUTYLLITHIUM (709 mL of 1.7 M) in pentane is then slowly added via a dropping funnel. After the addition is complete, the reaction mixture is allowed to warm TO-30C and stirred, at that temperature, for 2 hours. The reaction mixture is cooled to-78C and an excess amount (100 g) of dry-ice is added. The reaction mixture is again allowed to warm TO-30C and stirring is continued for 2 hours AT-30C and then at room temperature overnight. The reaction is quenched by addition of saturated aqueous ammonium chloride (500 mL). The mixture is partitioned between 1 N HCI (500 mL) and EtOAc (500 mL). The organic layer is washed with brine (400 mL), dried (MGS04) and concentrated by rotary evaporator to give crude product which is purified by flash chromatography (10: 1 HEXANES/METHANOL) to give 4- (BOC-amino)-5- TRIFLUOROMETHYLBENZOIC ACID (m. p. 197-198C). 2- (BOC-AMINO)-5-TRIFLUOROMETHYLBENZOIC acid, obtained above (120 G) is dissolved in absolute ethanol (200 mL) and treated with 3 N HCI (80 mL). The reaction mixture is heated to reflux temperature for 3 hours and then cooled to room temperature. Most of the ethanol is removed by rotary evaporator and the pH of the remaining solution adjusted to pH 7 with 2 N NAOH solution. The mixture is extracted with EtOAc (500 mL), the organic layer is washed with brine (250 mL), dried (MGS04) and the solvent removed by rotary evaporator. The residue is purified by trituration with hexanes and filtration to give 5- trifluoromethylanthranilic acid (m. p. 191-192C). 5-Trifluoromethylanthranilic acid (43 G, 0.21 mol) is suspended in a mixture of concentrated HCI (40 mL) and water (240 mL), cooled to 0C and stirred. Sodium nitrite (18 g, 0.26 mol) is dissolved in water (50 mL) and slowly added taking care to maintain the temperature of the reaction mixture below 5C. Stirring is continued at 0C for 30 minutes. Potassium iodide (65 G, 0.39 mol) is dissolved in a mixture of concentrated H2SO4 (15 mL) and water (100 mL) and the solution is added dropwise to the reaction mixture while keeping the temperature below 10C. The mixture is then heated to 100C and stirred for 2 hours. After cooling to room temperature, the mixture is partitioned between EtOAc (750 mL) and saturated sodium bisulfite solution (500 mL). The organic layer is washed again with saturated sodium bisulfite solution (500 mL) and then brine (500 mL), dried (MGS04) and concentrated by rotary evaporator to give 5-trifluoromethyl-2-iodobenzoic acid (m. p. 171- 172C). 5-Trifluoromethyl-2-iodobenzoic acid (50 g, 158 MMOL) is dissolved in anhydrous THF (200 mL) and cooled in an ice-salt bath until the temperature REACHES-5C. Borane-THF complex is added dropwise as a 1.0 M solution in THF (350 mL, 350 MMOL) AT-5C. After addition is complete, the reaction mixture is slowly warmed to room temperature and stirred for 12 hours. Water (40 mL) is carefully added dropwise (foaming) and the reaction mixture stirred for 30 minutes. Additional water (350 mL) is added and the mixture is concentrated by rotary evaporator to remove most of the THF. Additional water (250 mL) is added to form a precipitate, which is isolated by filtration to give 5-trifluoromethyl-2-iodobenzyl alcohol (m. p. 81-82C). 5-Trifluoromethyl-2-iodobenzyl alcohol (45 g, 0.15 mol) is dissolved in anhydrous ET20 (400 mL) and treated with phosphorous tribromide (41 mL, 0.15 mol) by dropwise addition. The reaction mixture is stirred at room temperature overnight and quenched by slow addition of water (150 mL). The organic layer is separated, washed with saturated aqueous NAHCO3 (250 mL), brine (250 mL), dried (MGS04) and concentrated by rotary evaporator to give 5-trifluoromethyl-2-iodobenzyl bromide as an oil. A solution of 5-trifluoromethyl-2-iodobenzyl bromide (55 G, 0.15 mol) in EtOH (200 mL) is stirred at room temperature and a solution of sodium cyanide (16 g, 0.33 mol) in water (60 mL) is added. The reaction mixture is heated to reflux temperature for 3 hours and then cooled to room temperature. Most of the ethanol is removed by rotary evaporator and the residue partitioned between EtOAc (500 mL) and water (200 mL). The organic layer is washed with brine (250 mL), dried (MGS04) and the solvent is removed by rotary evaporator. The residue is purified …

The synthetic route of 702641-04-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/48314; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene, molecular formula is C8H8I2O2, 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. HPLC of Formula: C8H8I2O2

Under an argon atmosphere, 15.6 g of compound 1 was dissolved in 100 mL of dichloromethane,And 8.18 mL of boron tribromide was added dropwise to the solution at -78 C.Wherein the molar ratio of compound 1, boron tribromide and methylene chloride is 1: 2.2: 40. The reaction was stirred for 16 hours,After completion of the reaction, the reaction solution was transferred to an ice-water mixture and stirred, suction-filtered and dried in vacuo to give a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 51560-21-5, its application will become more common.

Reference:
Patent; Shaanxi Normal University; Fang, Yu; Qi, Yanyu; Sun, Xiaohuan; Chang, Xingmao; Cui, Hong; He, Meixia; Wang, Gang; (22 pag.)CN104893714; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com