Month: August 2021

Related Products of 3032-81-3, These common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-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.

General procedure: A solution of 4-cyano-1H-imidazole (1000 mg, 10.74 mmol), 4-iodo -2-(trifluoromethyl)pyridine (3800 mg,14 mmol), (1R,2R)-N1,N2-dimethyl cyclohexane -1,2-diamine (150 mg, 1.07 mmol), CuI (200 mg, 1.07 mmol) and Cs2CO3 (7000 mg, 21.5 mmol) in 20 mL anhydrous DMF was stirred at 100 oC for 2 hours. The reaction mixture was cooled to room temperature and poured into 200 mL water. The mixture was extracted with ethyl acetate (80 mL*3). The organic layer were combined, washed by brine, dried by Na2SO4 and evaporated. The crude product was purified by silica flash column to afford compound 2 as white solid(1.5 g, 59percent yield).

Statistics shows that 1,3-Dichloro-5-iodobenzene is playing an increasingly important role. we look forward to future research findings about 3032-81-3.

Reference:
Article; Zheng, Qiangang; Chen, Ziqi; Wan, Huixin; Tang, Shuai; Ye, Yan; Xu, Yuan; Jiang, Lei; Ding, Jian; Geng, Meiyu; Huang, Min; Huang, Ying; Bioorganic and Medicinal Chemistry Letters; vol. 28; 23-24; (2018); p. 3808 – 3812;,
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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C7H6BrIO

Step 1: An oven-dried flask equipped with a magnetic stir bar was charged with l-bromo-4- chloro-2-fluoro-5-methoxy-benzene (100 mg, 0.42 mmol), (4-methoxyphenyl)boronic acid (69.8 mg, 0.46 mmol) and [l,l’-bis(diphenylphosphino)ferrocene] dichloropalladium(II) complex with dichloromethane (17.1 mg, 0.021 mmol). The flask was sealed with a rubber septum, and then evacuated and backfilled with argon (repeated a total of 3 X). l,4-Dioxane (1.0 mL) and aqueous 1 M K2CO3 (0.5 mL, 0.5 mmol) were added and the reaction was heated to 90 C for 2 h. The reaction was cooled to room temperature, diluted with water (5 mL), and extracted with EtOAc (3 X). The combined organic phases were dried over Na2S04, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with a EtOAc/hexanes gradient (0-10% EtOAc) to yield l-chloro-5-fluoro-2-methoxy-4-(4- methoxyphenyl)benzene (89.2 mg, 80%) as an off white solid. (1337) MS m/z 267.8 [M+H]+; 1H NMR (CDCL) d: 7.39 (dd, /= 8.8, 1.6 Hz, 2H), 7.13 (d, /= 9.5 Hz, 1H), 6.92 (d, J= 8.8 Hz, 2H), 6.85 (d, J= 6.9 Hz, 1H), 3.85 (s, 3H), 3.79 (s, 3H).

The synthetic route of 755027-18-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PTC THERAPEUTICS, INC.; SYDORENKO, Nadiya; ALAM, Md Rauful; ARNOLD, Michael A.; BABU, Suresh; BHATTACHARYYA, Anuradha; CHEN, Guangming; GERASYUTO, Aleksey I.; KARP, Gary Mitchell; KASSICK, Andrew J.; MAZZOTTI, Anthony R.; MOON, Young-Choon; NARASIMHAN, Jana; PATEL, Jigar; TURPOFF, Anthony; WOLL, Matthew G.; YAN, Wuming; ZHANG, Nanjing; (0 pag.)WO2020/5873; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 340825-13-0, 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. 340825-13-0, name is 6-Iodo-3,4-dihydronaphthalen-1(2H)-one, This compound has unique chemical properties. The synthetic route is as follows.

A 200 mL round bottom flask was charged with Compound 6 (4.1 g, 15 mmol),Methanol (100 mL) was added, and at 0 C. under ice cooling,Sodium borohydride (850 mg, 22.5 mmol) was gradually added,The mixture was stirred at 0 C. for 3 hours.The excess sodium borohydride was neutralized with dilute hydrochloric acid, saturated brine was added,Extraction was carried out 5 times with ethyl acetate (50 mL).The extract was washed once with ammonium chloride (100 mL)Subsequently, the solution was washed twice with saline (100 mL), dried over sodium sulfate.The filtrate was concentrated, as a pale red solid,Compound 7 was obtained (yield 3.93 g, yield 95.5%).This was used as it was for the next reaction without further purification.

The chemical industry reduces the impact on the environment during synthesis 6-Iodo-3,4-dihydronaphthalen-1(2H)-one. I believe this compound will play a more active role in future production and life.

Reference:
Patent; RICOH COMPANY LIMITED; GOTO, DAISUKE; YAMAMOTO, SATOSHI; MIYAGAWA, SATOSHI; KATO, TAKUJI; MOHRI, MASATAKA; NAKANOTANI, HAJIME; (65 pag.)JP6146001; (2017); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 4387-36-4, 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. 4387-36-4, name is 2-Iodobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows.

A modified literature procedure was employed. ADDIN EN.CITE Finnegan1958951959517Finnegan, William G.Henry, Ronald A.Lofquist, RobertAn Improved Synthesis of 5-Substituted TetrazolesJournal of the American Chemical SocietyJournal of the American Chemical SocietyJ. Am. Chem. Soc.J Am Chem Soc3908-3911801519581958/08/01American Chemical Society0002-7863https://doi.org/10.1021/ja01548a02810.1021/ja01548a0281In a 500 mL round bottom flask equipped with magnetic stir bar, 2-iodobenzonitrile (10.0 g, 0.0436 mol), NH4Cl (4.67 g, 0.0872 mol) and NaN3 (5.67 g, 0.0872 mol) were added, followed by DMF (200 mL). Subsequently, the flask wassealed with a glass stopper and submerged in an oil bath at 130 C. Thereaction mixture was stirred vigorously for 20 h and the flask was allowed to cool down to ambient temperature. Then, distilled water (150 mL) was added to the reaction mixture, followed by 10% (v/v)aqueous HCl solution, until pH reached the value of 1-2. The product and unreacted 2-iodobenzonitrile precipitated, and was filtered, and washed with water several times. Then, 0.1 N NaOH (500 mL) was added to the precipitate to get a suspension. This suspension wasfilteredto remove the unreacted 2-iodobenzonitrile and the filtrate was collected. Subsequently, 10% (v/v) aqueous HCl solution was added to the filtrate until pH reached the value of 1-2 and the product precipitated. The precipitate was filtered, and washed with water several times, and thenwith diethyl ether. The obtained product was dried under vacuum at 40 C for 24 h and theyield was determined (8.9 g, 75%). 1H NMR (400 MHz, (CD3)2SO): delta 8.10 (d, J = 7.9 Hz, 1H), 7.60 (d, J = 4.1 Hz, 2H), 7.42 – 7.30 (m, 1H).13C{1H} NMR (101 MHz, (CD3)2SO): delta 156.97, 140.26, 132.87, 131.73, 131.01, 128.94, 98.11.

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

Reference:
Article; Vaish, Avichal; Sayala, Kapil Dev; Tsarevsky, Nicolay V.; Tetrahedron Letters; vol. 60; 35; (2019);,
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. 14452-30-3, name is 1-(3-Iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1-(3-Iodophenyl)ethanone

Step A: 4-(3-Iodo-phenyl)-2,4-dioxo-butyric acid methyl ester Sodium hydride (60% oil dispersion, 4.9 g, 123 mmol) was added in portions to a solution of 3-iodoacetophenone (25.18 g, 102.3 mmol) and dimethyl oxalate (14.5 g, 123 mmol) in DMF (125 mL) at 0 C. The mixture stirred at room temperature for 1 hour and was then heated at 115 C. for 1 h. After cooling, the mixture was treated with 3 M HCl and then diluted with ethyl acetate. The organic layer washed three times with water and saturated brine, dried over anhydrous sodium sulfate, filtered and concentrated. Chromatography on silica gel, 0-10% ethyl acetate in hexanes, afforded 24.2 g of the subtitle compound (71.3% yield) as a yellow solid which was used directly in the next step.

According to the analysis of related databases, 14452-30-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AstraZeneca AB; NPS PHARMACEUTICALS, INC.; US2007/259895; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 13194-69-9,Some common heterocyclic compound, 13194-69-9, name is 2-Iodo-5-methylaniline, molecular formula is C7H8IN, 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.

The corresponding imidazopyridine (0.2 mmol) was added sequentially to a 25 ml Schlenk tube filled with oxygen and equipped with a magnetic stirrer at room temperature.Cuprous iodide (0.04 mmol), 2-iodo-5-methylaniline (0.3 mmol), 1,10-azaphenanthroline (0.04 mmol), sodium carbonate (0.6 mmol), and carbon disulfide were added by syringe under oxygen conditions ( 0.6 mmol), DMF (2.0 mL), and the reaction tube was stirred in a 120 C oil bath for 9 hours. The obtained solution was cooled to room temperature, 2 mL of deionized water was added to the reaction liquid, and the mixture was uniformly mixed. Each time, 3 mL of ethyl acetate was used as an extracting agent, and the crude product was extracted from the reaction liquid by a liquid separation extraction operation, and the extract was combined. The solvent was removed by a rotary evaporator; the residue was purified on a silica gel column (yield: 200 mesh to 300 mesh, eluted with petroleum ether/ethyl acetate (7:1 v/v)) to give the desired product 55.2 mg. The yield was 74%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-5-methylaniline, its application will become more common.

Reference:
Patent; Qingdao University of Science and Technology; Yang Daoshan; Yan Qiuli; (17 pag.)CN110294757; (2019); A;,
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. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 1-Iodo-3-(trifluoromethyl)benzene

General procedure: A mixture of cobalt(II) oxalate dihydrate(Sigma-Aldrich, 0.294 mmol), Cs2CO3 (2.94 mmol), pyrrolidinoneor aliphatic amide (1.47 mmol), DMEDA (0.588 mmol),distilled H2O (0.3 mL) and aryl halide (2.205 mmol) were addedto an 8.0-mL reaction vial fitted with a Teflon-sealed screw cap.The reaction mixture was stirred under air in a closed system at120 C and 130 C, respectively for 24 h. The heterogeneousmixture was subsequently cooled to r.t. and diluted withCH2Cl2. The combined organic extracts were dried over anhydNa2SO4, filtered and the solvent was removed under reducedpressure. The crude product was loaded into the column usingminimal amounts of CH2Cl2 and was purified by silica gel column chromatography to afford the N-arylated product. Theidentity and purity of products were confirmed by 1H NMR and13C NMR spectroscopic analysis.

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

Reference:
Article; Tan, Bryan Yong-Hao; Teo, Yong-Chua; Synlett; vol. 26; 12; (2015); p. 1697 – 1701;,
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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, A new synthetic method of this compound is introduced below., name: 4-Iodo-1,2-dimethylbenzene

(37-1) Synthesis of 3-(3,4-dimethylphenyl)-2-propyne-1-ol (compound 37-1) [Show Image] A mixture of 1-iodo-3,4-dimethylbenzene (5.00 g), copper(I) iodide (82.1 mg), triphenylphosphine (283 mg), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (446 mg), propargyl alcohol (1.40 ml), diisopropylethylamine (15.0 ml) and tetrahydrofuran (100 ml) was stirred at room temperature for 5 hr. The reaction mixture was added to brine, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=98:2 – 80:20) to give the object product (2.12 g) as a brown oil. 1H-NMR(CDCl3) delta (ppm): 1.64(1H, t, J=6.2Hz), 2.23(3H, s), 2.26(3H, s), 4.48(2H, d, J=6.0Hz), 7.07(1H, d, J=7.7Hz), 7.18(1H, d, J=7.7Hz), 7.22(1H, 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; Mitsubishi Tanabe Pharma Corporation; EP2168944; (2010); 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. 13421-00-6, name is 5-Chloro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., name: 5-Chloro-2-iodobenzoic acid

The 1-[2,8-dichloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-piperazine (melting point 120-122 C.) used as the starting material can be prepared from 5-chloro-2-iodo-benzoic acid and 4-chloro-phenol in the manner described in Example 1, via the following intermediates:

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; US4032525; (1977); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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: C6H3Cl2I

General procedure: To 4-amino-l-(4-methoxybenzyl)-lH-imidazo[4,5-c]pyridine-2-thiol (103) (50 mg, 0.174 mmol) was added respective iodine (0.348 mmol), neocuproine hydrate (3.6 mg, 0.0174 mmol), Cul (3.3 mg, 0.0174 mmol), sodium tert-butoxide (25 mg, 0.261 mmol) and lastly DMF (5 mL) and the reaction mixture was stirred at 1 10°C for 24 hours. Then, the solvent was removed under reduced pressure and the crude product was purified by preparatory TLC (CH2Cl2:MeOH-NH3 (7N), 10: 1) to afford desired compounds 104a-c. [0457] 2-((3,5-dichlorophenyl)thio)-l-(4-methoxybenzyl)-lH-imidazo[4,5-c]pyridin-4-amine (104a). Obtained as pale yellow solid 39percent yield. LCMS found m/z 430.97 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3032-81-3, its application will become more common.

Reference:
Patent; MEMORIAL SLOAN-KETTERING CANCER CENTER; CHIOSIS, Gabriela; YAN, Pengrong; PATEL, Pallav; PATEL, Hardik J.; TALDONE, Tony; YANG, Chenghua; SUN, Weilin; OCHIANA, Stefan; WO2015/23976; (2015); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com