Tag: M.W=300-400

Synthetic Route of 2034-22-2, 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. 2034-22-2, name is 2,4,5-Tribromoimidazole belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a single-necked flask was added 2,4,5-tribromoimidazole (49 g, 161 mmol)Sodium sulfite (101.5 g, 806 mmol)And water (500 ml) were added and stirred at 110 C for 6 h,Ethyl acetate was added,The organic layers were combined and dried over anhydrous sodium sulfate,Rotate the ethyl acetate to give compound 6 (20.5 g, yield 89%)

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, 2,4,5-Tribromoimidazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hinova Pharmaceuticals Inc.; Fan, Lei; Chen, Ke; Li, Xinghai; Chen, Yuanwei; (24 pag.)CN106256830; (2016); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

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. 15469-97-3, name is 1-Trityl-1H-imidazole, A new synthetic method of this compound is introduced below., Product Details of 15469-97-3

A cooled (-78°C) yellow solution of 1-(triphenylmethyl)imidazole (25.000 g; 80.542 mmol) in anhydrous THF (750 ml) was treated dropwise (in 55 min.) with a 1.6M solution of butyllithium in hexanes (55.35 ml; 88.560 mmol). After addition, the resulting pink homogeneous solution was further stirred at -78°C, under nitrogen, for 30 min. before a solution of anhydrous DMF (6.8 ml; 88.186 mmol) in anhydrous THF (40 ml) was added dropwise (in 40 min.). The resulting mixture was additionally stirred at -78°C, under nitrogen, for 1 h before aq. sat. NH4CI (50 ml) was added dropwise. Ether (300 ml) and water (400 ml) were successively added, and this mixture was allowed to warm-up to rt. The yellow organic layer was additionally washed with water (300 ml), dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure. The crude was purified by FC (DCM / MeOH = 30 / 1 ) to give the pure product 1 -trityl-1 H-imidazole-2- carbaldehyde as a pale yellow solid which was further dried under HV (20.660 g; 76percent). LC-MS: tR = 1.03 min.; [M+H]+: no ionisation.

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; ACTELION PHARMACEUTICALS LTD; WO2008/78291; (2008); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Synthetic Route of 2034-22-2, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2034-22-2 name is 2,4,5-Tribromoimidazole, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Step 1. 2,4,5-Tribromo-l-methyl-lH-imidazole (0975) [00314] To a suspension of sodium hydride (0.787 g, 19.69 mmol) in DMF (15 mL) was added 2, 4, 5-tribromo-lH-imidazole (5 g, 16.41 mmol) in DMF (10 mL) at ambient temperature. The mixture was stirred at 50 C for 1 h, cooled to 0 C, and treated with methyl iodide (1.128 ml, 18.05 mmol). The mixture was warmed to 50 C and stirred 16 h, the DMF was removed under reduced pressure and EtOAc was added. The mixture was washed with water, dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (eluting with a gradient of 10-80% EtOAc/hexanes) afforded 4.87 g (94%) of 2,4,5-tribromo-l -methyl- lH-imidazole. 1H MR (300 MHz, CDC13) delta 3.62 (s, 3H). MS (ESI) m/z 316.77 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,4,5-Tribromoimidazole, and friends who are interested can also refer to it.

Reference:
Patent; FORMA THERAPEUTICS, INC.; BUCKMELTER, Alexandre Joseph; IOANNIDIS, Stephanos; FOLLOWS, Bruce; GUSTAFSON, Gary; WANG, Minghua; CARAVELLA, Justin A.; WANG, Zhongguo; FRITZEN, Edward L.; LIN, Jian; (414 pag.)WO2017/87837; (2017); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

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. 143722-29-6, name is 1-(4-Bromobenzyl)-2-butyl-4-chloro-1H-imidazole-5-carbaldehyde belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 1-(4-Bromobenzyl)-2-butyl-4-chloro-1H-imidazole-5-carbaldehyde

Example 3. Preparation of 3-(4-bromobenzyl-2-butyl-5-chloro-3h-imidazol-4-yl)-methanol (II) A round-bottom flask is loaded with 0.6 g of 3-(4-bromobenzyl)-2-butyl-5-chloro-3H-imidazole-4-carboxaldehyde and 5 ml of methanol. The mixture is cooled to 0-5C and added with 78 mg of sodium borohydride. Stirring is continued for 30′, then 5 ml of a saturated ammonium chloride solution are added. The solvent is evaporated off and the residue is taken up with 10 ml of ethyl acetate. After two washings with 5 ml of water the organic phase is evaporated to give 480 mg of a crude residue, which is crystallized from ethanol-water. 320 mg of 3-(4-bromobenzyl-2-butyl-5-chloro-3H-imidazol-4-yl)-methanol are obtained as colourless crystals.

The synthetic route of 143722-29-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dipharma S.p.A.; EP1548009; (2005); A2;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Reference of 2034-22-2, 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. 2034-22-2, name is 2,4,5-Tribromoimidazole belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

General procedure for the synthesis of AB1 To a stirred solution of 2,4,5-tribromoimidazole (1.0 g, 3.28 mmol) in tetrahydrofuran (15.0 mL) was added NaH (60% dispersion in paraffin, 0.20 g, 4.92 mmol) under ice-bath. After 10 min, chloromethyl methyleter (0.30 mL, 3.94 mmol) was added slowly. The reaction mixture was allowed to room temperature and further stirred for 1.5 hours. The reaction mixture was quenched with water (20 mL) and extracted with EtOAc (20 mL x 2). The organic layer was dried over anhydrous MgS04 and concentrated in vacuo to give AB1.

The synthetic route of 2,4,5-Tribromoimidazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INSTITUT PASTEUR KOREA; TERRAMARK MARKENCREATION GMBH; KIM, Jaeseung; KANG, Sunhee; KANG, Juhee; LEE, Sumi; SEO, Jeong Jea; SEO, Mooyoung; (156 pag.)WO2015/193506; (2015); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Application of 15813-09-9, These common heterocyclic compound, 15813-09-9, name is 4,5-Diiodo-1H-imidazole, 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.

To a solution of 4,5-diiodo-1H-imidazole (2.0 g, 5.9 mmol) in DMF (45 mL) was added NaH (60% in mineral oil, 356 mg, 8.91 mmol). The mixture was stirred at RT for 30 min, then treated with 2-(2-bromoethyl)isoindoline-1,3-dione (2.33 g, 8.91 mmol). The mixture was stirred at 60 C. overnight, then allowed to cool to RT and poured into water (30 mL). The precipitated solid was collected and dried to give the title compound as a white solid (1.72 g, 59%). MS (ES+): C13H9I2N3O2 requires: 493, found: 434 [M+H]+.

The synthetic route of 15813-09-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Board of Regents, The University of Texas System; LE, Kang; SOTH, Michael J.; JONES, Philip; CROSS, Jason Bryant; CARROLL, Christopher L.; MCAFOOS, Timothy Joseph; MANDAL, Pijus Kumar; US2019/298729; (2019); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Electric Literature of 29914-81-6, 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. 29914-81-6, name is 1,3-Bis(1H-benzo[d]imidazol-2-yl)benzene belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

c, 2.6 mmol of 1, 14.5 mmol KOH and 2 mL of 1-iodo-n-hexane were dissolved in 30 mL of acetonitrile, refluxed for 24 hours, the solvent was removed to obtain a brown oil, dissolve with chloroform, and extracted and washed with distilled water 9 to 10 times. The filtrate was removed and the obtained brown solution was concentrated to 3 to 5 mL, and subjected to column chromatography with 100 to 200 mesh silica gel as the stationary phase and ethyl acetate as the eluent, Rf of the product was 0.7 to 0.8, to obtain dibenzimidazole phenyl complex 2 (yellow-white solid, yield 93%).

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, 1,3-Bis(1H-benzo[d]imidazol-2-yl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Guangzhou Yuxin Intelligent Science And Technology Institute Co., Ltd.; Xi Yanan; Hu Shujin; (19 pag.)CN110950912; (2020); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Reference of 33016-47-6, 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 33016-47-6 as follows.

E (R)-N-[1-(Phenylmethyl)-4-[1-(triphenylmethyl)-1H-imidazol-4-yl]-3-butenyl]benzenesulfonamide A solution of compound D (400 mg, 0.63 mmol) and 1-trityl-4-formylimidazole (320 mg, 0.94 mmol) in methylene chloride was dried over MgSO4. The solids were filtered and the filtrate evaporated to dryness. The white foam residue was diluted with of THF (24 mL) and 3A molecular sieves added. After 1 hour, a solution of lithium bis(trimethylsilyl)amide (1.4 mL, 1M) in THF was added dropwise. After 1 hour, the mixture was filtered and the filtrate was concentrated in vacuo. The residue was diluted with ethyl acetate and the solution washed with brine, dried (MgSO4) and concentrated. The resulting residue was purified by flash chromatography on silica gel. Elution with 40% ethyl acetate in hexane afforded (108 mg) of the title compound, and (149 mg) of the Z-isomer (Combined yield 67%). MS; (M+H)+=610.

According to the analysis of related databases, 33016-47-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bristol-Myers Squibb Company; US6387926; (2002); B1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Application of 2034-22-2,Some common heterocyclic compound, 2034-22-2, name is 2,4,5-Tribromoimidazole, molecular formula is C3HBr3N2, 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.

STAGE 1: 1-((6-chloro-1,3-benzodioxol-5-yl)-methyl)-2,4,5-tribromo-1H-imidazole 25 g of 2,4,5-tribromoimidazole is introduced into 500 ml of dimethylformamide and 4.3 g of sodium hydride is added. Agitation is maintained for 10 minutes at ambient temperature. Next 18.4 g of 6-chloro piperonyl chloride, then 25 g of sodium iodide are added to the reaction medium and agitation is continued for 15 minutes at ambient temperature. The reaction medium is finally poured into 3 litres of water, separated, washed abundantly with water, then successively with 250 ml of ethanol, 250 ml of isopropanol, then finally with 250 ml of isopropyl ether. After drying, 31.5 g of expected product (cream solid) is collected M.p.=225 C. IR CHCl3 (cm-1) Absence of =C–NH

The synthetic route of 2034-22-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoechst Marion Roussel; US6143774; (2000); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

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. 3543-74-6, name is Ethyl 4-(5-(bis(2-hydroxyethyl)amino)-1-methyl-1H-benzo[d]imidazol-2-yl)butanoate, A new synthetic method of this compound is introduced below., COA of Formula: C18H27N3O4

Example 20: Preparation of crude Bendamustine hydrochloride (form B) [00103] A 5 L bottle was charged with 197 g of phosphorus oxychloride. The contents of the bottle were heated to 50 0C and 150 g of ethyl 4-{5-[bis(2- hydroxycthyl)amino]-l -methyl- lH-benzimidazol-2-yl}butanoatc(“BBOH”) dissolved in 600 ml of dichloromethane was added. Reaction mixture was stirred at 75-85 0C for 4-5 hours. The reaction mixture was then cooled to room temperature and diluted with 450 ml dichloromethane to form a solution. Then the solution was decomposed with 900 ml of 21 % hydrochloric acid and then this reaction mixture was heated at 92 – 96 C for 5-6 h. The resulting solution was then cooled, and its pH was adjusted with 50 % sodium hydroxide to a pH of 1.4 – 1.6 at 0 – 200C. The product crystallized and the mixture was stirred 30 – 60 minutes at 0-100C. The crude Bendamustine was separated by filtration and the filter cake was washed three times with 600 ml of cold dilute hydrochloric acid (1 :20), then three times with 600 ml of cold water, and then three times with 600 ml of ethyl acetate . The filter cake was then dried in wet (relative humidity over 30 %) nitrogen to give 144 g of crude bendamustine hydrochloride.

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; PLUS CHEMICALS SA; TEVA PHARMACEUTICALS USA, INC.; KUCHAR, Martin; KORYTAKOVA, Romana; POSPISILIK, Karel; GAVENDA, Ales; VRASPIR, Pavel; JEGOROV, Alexandr; WO2010/144675; (2010); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem