Iodides-buliding-blocks

Related Products of 35453-19-1, A common heterocyclic compound, 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, molecular formula is C8H4I3NO4, 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.

5-Amino-2,4,6-triiodoisophathalic acid (15.38 g, 27.5 mmol, 1.0 equiv.) was refluxed in SOCl2 ( 10OmL, 1.37 mol, 50.0 equiv.) for 4 hours. The volatiles were removed in vacuo and the resultant dark yellow residue was dissolved in ethyl acetate (300 mL). The organic layer was washed with sat. NaHCO3 (3 x 150 mL), water (3 x 150 mL) and brine (150 mL) and concentrated in vacuo. The residue was dissolve in toluene and passed through a short pad of silica, dried (MgSO4) and concentrated in vacuo to yield the title compound as a beige solid (10.74 g, 66 %). IR spectrum in KBr disc/cm”1: v(N-H) 3370, 3470; V(C=O) 1770, 1798

The synthetic route of 35453-19-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IMPERIAL INNOVATIONS LIMITED; KINGS COLLEGE LONDON; GUYS AND ST THOMAS NHS FOUNDATION TRUST; WO2007/26140; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 450412-29-0, A common heterocyclic compound, 450412-29-0, name is 1-Bromo-3-fluoro-2-iodobenzene, molecular formula is C6H3BrFI, 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.

28.3 g (100 mmol, 1.0 eq.) m-bromoiodobenzene and 25.8 g m-bromoaniline (150 mmol, 1.5 eq.)It was placed in a dry 3 L three-necked flask, and then dried and degassed 1100 ml of toluene was added as a solvent.Nitrogen gas was passed for 15 minutes. Add 2.9g (15% mol) of cuprous iodide,5.9 g (30% mol) of 1,10-phenanthroline and 63.7 g (300 mol, 3 eq.) potassium phosphate.The temperature was raised to 110 C and the reaction was carried out for 18 hours. After the reaction is completed, cool to room temperature, suction filtration,Rotating to remove the solvent,Recrystallization with toluene and ethanol,27.8 g of intermediate L were obtained,The yield was 85%.

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

Reference:
Patent; Nanjing Gao Guang Semiconductor Materials Co., Ltd.; Jin Zhenyu; Qian Chao; Wang Xiaowei; Dai Peipei; (49 pag.)CN108164511; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 19094-56-5, 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. 19094-56-5 name is 2-Chloro-5-iodobenzoic acid, 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.

1. Synthetic routeWherein, the condition (b) is (COCl)2, CH2Cl2, DMF/Pyr, CH3OH, 2 to 3 h, r.t.2, the synthesis step(1) The compound B (B1,B2,B3) of the compound of Example 1 after purification (1 g, 3.16 mmol, 3.16 mmol, 3.54 mmol) was weighed under nitrogen, after adding 20 mL of ultra-dry anhydrous dichloromethane (DCM) and stirring to dissolve completely, add three times the amount of oxalyl chloride (9.48 mmol, 9.48 mmol, 10.62 mmol) and stir for 20-30 min; (2) Under nitrogen protection, 0.1 mL of anhydrous grade N,N-dimethylformamide (DMF) was added. After reacting for 1 h at room temperature, The reaction activated product is vacuum dried, And minimize external air entering the reaction device during operation; Use nitrogen as a shielding gas and add ultra-dry dichloromethane solvent. After stirring and dissolved at room temperature, Add twice the amount of anhydrous pyridine (6.32 mmol, 6.32 mmol, 7.08 mmol), The reaction was stirred for 30 min; finally, twice the amount of ultra-dry methanol (6.32 mmol, 6.32 mmol, 7.08 mmol) was added under a nitrogen atmosphere at room temperature. The reaction was stirred for 3 h or more; the reaction end point was detected by TLC [developing agent: V (petroleum ether)/V (ethyl acetate) = 20/1];(3) After the reaction is completed, it is extracted by washing with ethyl acetate. And dried over anhydrous MgSO4, filtered and concentrated. The crude product of the intermediate C(C1,C2,C3) was obtained, purified by silica gel column chromatography [eluent: V ( petroleum ether) / V (ethyl acetate) = 50/1] obtaining the compound intermediate C (C1,C2,C3), colorless oily liquid with yields of 72%, 58% and 63%, respectively.

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

Reference:
Patent; Guangdong University of Technology; Zhao Suqing; Zhang Bingjie; Feng Dongyan; Zhong Yingying; Huang Jinqu; Wu Ke; Ling Huaying; Tan Qiting; Chen Yanting; Zhao Jiawei; Ma Zhuolin; Jiang Zhengyun; Yang Yang; Zhu Qiuyan; Hong Weiqian; (37 pag.)CN110143869; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 61272-76-2, 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. 61272-76-2, name is 4-Fluoro-2-iodoaniline, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: 2-Iodoaniline 2a (65.7 mg, 0.3 mmol), Cu(OAc)2 (6 mg, 10percent), KOtBu (101 mg, 0.9 mmol), DMAc (1.0 mL) were mixed in a Schlenck tube and then to the mixture was added 2-(phenylethynyl)benzonitrile1a (74 mg, 0.36 mmol) under N2. The reaction mixture was stirred for 12 h at 120 ¡ãC under N2. After the reaction was completed (monitored by TLC), the reaction mixture was then diluted with water and extracted with ethyl acetate. After the combined organic layers were washed with brine, dried over Na2SO4, and concentrated under reduced pressure, the residue was purified by flash column chromatography on silica gel using petroleum ether/ethyl acetate as eluent to afford the pure product 3

The chemical industry reduces the impact on the environment during synthesis 4-Fluoro-2-iodoaniline. I believe this compound will play a more active role in future production and life.

Reference:
Article; Liu, Xiaodong; Deng, Guobo; Liang, Yun; Tetrahedron Letters; vol. 59; 29; (2018); p. 2844 – 2847;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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 10 mL flask equipped with a Teflon valve was charged with a magnetic stir bar, CuI (2 mg, 1molpercent), Heteroarylamine (1.5 mmol), KOtBu (224 mg, 2.0 mmol), solid aryl halides (1.0 mmol). The tube was evacuated and backfilled with argon. Under a counter flow of argon, dioxane (1.5mL), aryl halides (1.0 mmol, if liquid) were added by syringe. The tube was sealed. The reaction mixture was allowed to stir at 110 ¡ãC (X=I) or 130 ¡ãC (X= Br) for 24 h. Then the mixture was cooled to room temperature and added 5.0 mL brine. Subsequently, the mixture was extracted with ethyl acetate. The organic layers were collected, dried over Na2SO4, filtered and the solvent was removed under vacuum. The residue was purified by column chromatography on silica gel.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Deping; Kuang, Daizhi; Zhang, Fuxing; Liu, Yang; Ning, Shunhua; Tetrahedron Letters; vol. 55; 51; (2014); p. 7121 – 7123;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 161949-50-4, name is 2-Chloro-5-iodoanisole, 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 161949-50-4, name: 2-Chloro-5-iodoanisole

2nd reaction step: 4-Chloro-3-methoxybenzeneboronic acid In a flame-dried flask, 1.93 g (79.2 mmol) of magnesium turnings were etched with a small crystal of iodine, and 50 ml of anhydrous ether were added. Then, under a nitrogen atmosphere, a solution of 20.0 g (79.2 mmol) 2-chloro-5-iodoanisole in 50 ml of anhydrous ether were added dropwise in such a way that the ether was kept boiling by the heat of reaction. After the addition was complete, the mixture was refluxed for 11/2 hours and then filtered through glass wool, with exclusion of moisture, into a dropping funnel. This Grignard solution and, synchronously but separately, 8.24 g (79.2 mmol) of trimethyl borate were added dropwise to 50 ml of anhydrous ether in a flame-dried flask under a nitrogen atmosphere at -60 to -70 C. The resulting suspension was then stirred at the stated temperature for one hour and, after it had warmed to about 20 C., acidified to pH 3 with 5% strength sulfuric acid. After separation of the phases, the aqueous phase was extracted three times with ether. The combined organic phases were dried over sodium sulfate and then concentrated. The residue was extracted by boiling three times with 100 ml of water each time. The aqueous phases were combined and cooled, when 4.6 g (32%) of colorless crystals separated out and were removed and dried under reduced pressure at 20-25 C. 1 H-NMR (270 MHz, in d6 -DMSO): delta [ppm]=3.90(s,3H), 7.39(s,2H), 7.56(s,1H), 8.2(s,br.,2H).

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-Chloro-5-iodoanisole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BASF Aktiengesellschaft; US5783522; (1998); 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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 460-37-7

Example 182Preparation of 4-((lR,3aS,5aR,5bR,7aR,llaS,llbR,13aR,13bR)-5a,5b,8,8,lla- pentamethyl-l-(prop-l-en-2-yl)-3a-((3,3,3-trifluoropropyl)amino)- 2,3,3a,4,5,5a,5b,6,7,7a,8,ll,lla,llb,12,13,13a,13b-octadecahydro-lH- cyclopenta[a]chrysen-9-yl)benzoic acidStep 1. Preparation of methyl 4-((lR,3aS,5aR,5bR,7aR, l laS, l lbR, 13aR, 13bR)- 5a,5b,8,8, 1 1 a-pentamethyl- 1 -(prop- 1 -en-2-yl)-3 a-((3,3 ,3 -trifluoropropyl)amino)- 2,3,3a,4,5,5a,5b,6,7,7a,8, l l, l la, l lb, 12, 13, 13a, 13b-octadecahydro-lH- cyclopenta[a]chrysen-9-yl)benzoate.To a sealable vial containing methyl 4-((lR,3aS,5aR,5bR,7aR, l laS,l lbR, 13aR, 13bR)-3a-amino-5a,5b,8,8, l la-pentamethyl- 1 -(prop- 1 -en-2-yl)-2,3,3 a,4,5,5a,5b,6,7,7a,8, 11 , 11 a, 1 lb, 12, 13, 13 a, 13b- octadecahydro-lH-cyclopenta[a]chrysen-9-yl)benzoate, HC1 (0.075 g, 0.129 mmol) was added potassium carbonate (0.036 g, 0.258 mmol). The mixture was diluted with DMF (1 mL) and l-iodo-3,3,3-trifluoropropane (0.045 mL, 0.388 mmol) was added. The vial was sealed and the mixture was heated to 75 C for 23h then was cooled to rt. LC/MS showed a mixture of starting material and product. An additional 0.045 mL of l-Iodo-3,3,3-trifluoropropane was added and the mixture and was heated to 75 C for 48h then was cooled to rt. LC/MS showed further progression, but the reaction was still not complete. An additional 0.045 mL of l-iodo-3,3,3-trifluoropropane was added and the mixture was heated to 75 C for 71h, then was cooled to rt and was concentrated under reduced pressure. The mixture was adsorbed to silica gel and was purified by flash chromatography using a 0-15% EtOAc in hexanes gradient with 0.1% ammonium hydroxide added to the mixture and a Thomson 12g silica gel column. The fractions containing the expected product were combined and were concentrated under reduced pressure to give methyl 4-((lR,3aS,5aR,5bR,7aR, l laS, l lbR, 13aR, 13bR)-5a,5b,8,8, l la-pentamethyl-l-(prop-l- en-2-yl)-3a-((3,3,3-trifluoropropyl)amino)-2,3,3a,4,5,5a,5b,6,7,7a,8, l l, l la, l lb, 12, 13, 13a, 13b-octadecahydro-lH- cyclopenta[a]chrysen-9-yl)benzoate (0.032 g, 0.044 mmol, 34.1 % yield) as a white foam. LCMS: m/e 640.6 (M+H)+, 2.15 min (method 2). XH NMR (500 MHz, chloroform-d) delta 7.92 (d, J=8.24 Hz, 2H), 7.19 (d, J=8.24 Hz, 2H), 5.28 (dd, J=1.53, 6.10 Hz, 1H), 4.70 (d, J=1.83 Hz, 1H), 4.59 (s, 1H), 3.90 (s, 3H), 2.60-2.73 (m, 2H), 2.56 (dt, J=5.34, 10.91 Hz, 1H), 2.21-2.32 (m, 2H), 2.09 (dd, J=6.41, 17.09 Hz, 1H), 1.68 (s, 3H), 1.07 (s, 3H), 0.98 (s, 6H), 0.92 (s, 3H), 0.92 (br. s., 3H), 0.84-2.01 (m, 21H).

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; REGUEIRO-REN, Alicia; LIU, Zheng; SWIDORSKI, Jacob; SIN, Ny; VENABLES, Brian Lee; SIT, Sing-Yuen; CHEN, Yan; CHEN, Jie; MEANWELL, Nicholas A.; WO2012/106190; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 61272-76-2, 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. 61272-76-2, name is 4-Fluoro-2-iodoaniline, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of 2-iodoaniline (0.5 mmol), CS2 (0.6 mmol), an amine (0.6 mmol), CuO nanoparticles (0.5 mmol), and KOH (1.5-2 mmol) in DMSO (3 mL) was stirred at 110 ¡ãC for 6 h. The cooled solution was partitioned between ethyl acetate and water, and the organic layer was washed with water and brine, and then dried over Na2SO4. After removal of the solvent in vacuo, the residue was purified by silica-gel chromatography to give the desired benzothiazole.

The chemical industry reduces the impact on the environment during synthesis 4-Fluoro-2-iodoaniline. I believe this compound will play a more active role in future production and life.

Reference:
Article; Satish; Reddy, K. Harsha Vardhan; Ramesh; Karnakar; Nageswar; Tetrahedron Letters; vol. 53; 20; (2012); p. 2518 – 2521;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 401-81-0, 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.

General procedure: To a resealable Schlenk tube, was added Cs2CO3 (2.0mmol), KSCN (1.5mmol) and MCM-41-2N-CuCl (110mg, 0.05mmol), and the reaction vessel was fitted with a rubber septum. The vessel was evacuated and back-filled with argon and this evacuation/back-fill procedure was repeated one additional time. The aryl iodide (1.0mmol) and water (3mL) were then added under a stream of argon. The reaction tube was quickly sealed and the contents were stirred while heating in an oil bath at 130C for 48h. After completion of the reaction, the reaction mixture was cooled to room temperature, extracted with ethyl acetate (3¡Á5mL), and filtered. The MCM-41-2N-CuCl complex was washed with distilled water (2¡Á5mL), ethyl acetate (2¡Á5mL), and Et2O (2¡Á5mL) and reused in the next run. The extract was concentrated under reduced pressure and the residue was purified by flash column chromatography on silica gel (petroleum/ethyl acetate=50:1 to 10:1) to provide the desired product.

The synthetic route of 1-Iodo-3-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Short Survey; Cai, Mingzhong; Xiao, Ruian; Yan, Tao; Zhao, Hong; Journal of Organometallic Chemistry; vol. 749; (2014); p. 55 – 60;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

1878-69-9, name is 2-(3-Iodophenyl)acetic acid, 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. HPLC of Formula: C8H7IO2

EXAMPLE A.4. Compound c-3 (127l): 4-(4-fluoro-3-(4-(2-(3-iodophenyl)acetyl)piperazine-l-carbonyl)- benzyl)phthalazin-l(2H)-one. A solution of 3-iodophenyl acetic acid (6.5 mg, 0.048 mmol), l-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC) (10.5 mg, 0.055 mmol), N-hydroxy succinimide (NHS) and 600 mu DM F was stirred for 30 min at room temperature. Then, 4-(4-fluoro-3-(piperazine-l-carbonyl)benzyl)- phthalazin-l(2H)-one (10 mg, 0.0275 mmol) was added to the solution and the mixture was stirred at room temperature overnight. The reaction was washed with 500 mu of H20 and extracted with 500 mu dichloromethane (DCM). The resulting organic solution was purified on silica gel, using a gradient elution from neat DCM to DCM/hexane 5:1 to obtain the desired product as a white solid (3 mg, 20% yield). 1H NMR (CDCI3) delta = 9,82 (s, 1H), 8.40-8.38 (m, 1H), 7.71-7.69 (m, 2H), 7.55-7.53 (m, 1H), 7.51-7.50 (m, 2H), 7.25-7.24 (m, 2H), 7.09-6.90 (m, 3H), 4.20 (s, 2H), 3.64-3.31 (m, 8H), 2.84 (s, 2H). LC-ESI-MS (+) m/z = 633.1 [M+Na+]+. HRMS-ESI [M+H+]+ m/z calculated for [C28H24FIN403]+ 611.0955, found 611.0948.

The synthetic route of 1878-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MEMORIAL SLOAN KETTERING CANCER CENTER; REINER, Thomas; LEWIS, Jason S.; WEBER, Wolfgang; RODRIGUEZ, Beatriz Salinas; CARNEY, Brandon; CARLUCCI, Giuseppe; (89 pag.)WO2016/33293; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com