Month: July 2021

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 58755-70-7 as follows. name: 1-Iodo-4-methoxy-2-nitrobenzene

To a solution of 4-iodo-3-nitroanisole (5g, 17.9 mmole) in 100 [ML METHANOL] was added [FECL3] (50mg, 0.3 mmole) and activated carbon (40 mg). The mixture was heated to reflux and hydrazine hydrate (1.75 [G,] 35 mmole) was added dropwise. The mixture was [REFLUXED] for an additional 8 hours and cooled to room temperature, filtered through Celite. The filtrate was concentrated and purified by column chromatography (eluting with 10% EtOAc in hexanes) to give 4.05 g product as pale yellow oil (91% [YILD). 1H NMR (300 MHZ, CDCL3) No. 7. ]47 [(1 H,] d, J = 8.7 Hz), 6.31 (1H, d, [J=] 2.8 [HZ),] 6.13 (1 H, dd, [J=] 2.8, 8.7 Hz), 3.73 (3H, s).

According to the analysis of related databases, 58755-70-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PFIZER INC.; WO2003/106462; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

34883-46-0, name is 1-Iodo-2-phenoxybenzene, 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. Product Details of 34883-46-0

(1)To 1-iodo-2-phenoxybenzene (2g, 6.8mmol)Triethylamine (20mL)Adding 4 methoxyphenylacetylene to the solution(0.98 g, 7.4 mmol), Pd(PPh3)2Cl2 (95 mg, 135 mumol), CuI (26 mg, 135 mumol).Under argon protection conditions,After the reaction was carried out for 10 h, triethylamine was removed under reduced pressure.The residue was extracted with ethyl acetate (20 mL×3) then water (10 mL)Wash twice with saturated brine (10 mL), dry over anhydrous sodium sulfate and filtered.The solvent was removed under pressure. The residue was purified by silica gel column chromatography eluting elut1-((4-Methoxyphenyl)ethynyl)-2-phenoxybenzene(1.7 g, 85% yield).

The synthetic route of 34883-46-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhongshan University Tumor Cure Center (Zhongshan University Affiliated Tumor Hospital ? Zhongshan University Tumor Institute); Wen Shijun; Huang Peng; Zhu Daqian; Tu Yalin; Luo Bingling; (28 pag.)CN108976248; (2018); 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. 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Fluoro-2-iodobenzoic acid

Step 1 : 15.1 (1 .50 g, 5.64 mmol) is dissolved in DCM (8.3 mL). Then oxalylchloride (5.6 mL, 1 1.3 mmol) is added followed by one drop of DMF and the mixture is stirred at RT for 1 h. The solvent is removed under reduced pressure. The residue is mixed with DCM (8 mL) and added at 0C to a mixture of B-3 (1 .04 g, 5.13 mmol) and DIPEA (3.9 mL, 22.6 mmol) in DCM (8 mL). (0378) The mixture is stirred for 12h at 20C. Water is added and the organic layer and washed with (0379) NH4CI (sat. aq. solution), KHC03 (sat. aq. solution) and water. The organic phase is dried and concentrated. The residue is purified by flash column chromatography (using a solvent gradient from 100% Cyclohexane to Cyclohexane/EA 8/2) to afford 0.91 g of 15.2.. ESI-MS: 451 [M+H]+; (0380) HPLC (Rt): 1 .17 min (method P).

The synthetic route of 52548-63-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; RIETHER, Doris; FERRARA, Marco; HEINE, Niklas; LESSEL, Uta; NICHOLSON, Janet Rachel; PEKCEC, Anton; SCHEUERER, Stefan; (69 pag.)WO2017/178341; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3930-83-4, The chemical industry reduces the impact on the environment during synthesis 3930-83-4, name is 2-Iodobenzamide, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of 2-iodobenzamide (3) or 2-bromonicotinamide (6) (2.0 mmol) in DMSO (3 mL), was added aldehyde (2.2 mmol), NaN3 (260 mg, 4.0 mmol), CuBr (29 mg, 0.2 mmol), and l-proline (46 mg, 0.4 mmol). The reaction mixture was stirred at 80 C under air. After disappearance of the reactant (monitored by TLC), water (30 mL) was added to the mixture, and then extracted with ethyl acetate (15 mL) for three times. The extraction was washed with saturated NaCl solution, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using petroleum ether/ethyl acetate (10:1 to 3:1) as the eluent to give the desired products 5 or 7.

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-Iodobenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Ting; Chen, Minglu; Yang, Lei; Xiong, Zhengxin; Wang, Yongwei; Li, Fei; Chen, Dongyin; Tetrahedron; vol. 72; 6; (2016); p. 868 – 874;,
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. 1829-28-3, name is Ethyl 2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of Ethyl 2-iodobenzoate

To a 2-dram vial with a PTFE-lined cap was charged with acetal 1o (30.1 mg, 0.0980 mmol), ethyl 2-iodobenzoate (111 mg, 0.402 mmol), NBE-CO2Me (23.1 mg, 0.152 mmol), Pd(TFA)2 (3.3 mg, 0.00994 mmol), TFA-Gly-OH (3.3 mg, 0.0193 mmol), AgOAc (66.0 mg, 0.395 mmol), and DCE (2.00 mL). The resulting mixture was heated to 100° C. and stirred for 24 h. After cooling to room temperature, ethylenediamine (0.100 mL) was added, and the resulting mixture was stirred at 23° C. for 2 h. The mixture was filtered through a plug of silica gel, eluting with EtOAc (30 mL), and the filtrate was concentrated under reduced pressure. The residue was purified by preparative TLC (2:1 hexanes/EtOAc eluent) to afford arylation product 3opmono (13.6 mg, 30percent yield, Rf=0.21 in 2:1 hexanes/EtOAc) as a yellow oil and arylation product 3opdi together with an unidentified impurity (6.0 mg total). (20percent recovery of starting material 1o was also observed in the crude NMR prior to purification.) The impure arylation product 3opdi was then dissolved in MeOH (2.00 mL), HCl (gas) was bubbled through the mixture until the pH 1, and the mixture was stirred at room temperature for 23 h. Saturated aq. Na2CO3 (5 mL) and water (10 mL) were then added, and the mixture was extracted with EtOAc (3×15 mL). The combined organic layers were washed with brine (15 mL) and dried over anhydrous Na2SO4. The solvent was concentrated by rotary evaporation, and the resulting residue was purified by preparative TLC (2:1 hexanes/EtOAc eluent) to afford biaryl alcohol 6opdi (3.3 mg, 8percent yield, Rf=0.21 in 2:1 hexanes/EtOAc) as a colorless oil. Monoarylation product (3opmono): 1H NMR: (400 MHz, CDCl3) delta 8.17 (d, J=8.5 Hz, 1H), 8.05 (s, 1H), 7.86 (d, J=7.2 Hz, 1H), 7.83 (d, J=8.2 Hz, 1H), 7.72 (app. t, J=7.7 Hz, 1H), 7.61-7.48 (m, 2H), 7.46-7.30 (m, 4H), 6.86 (d, J=8.4 Hz, 1H), 6.32 (s, 1H), 5.40 (d, J=13.2 Hz, 1H), 5.23 (d, J=13.2 Hz, 1H), 4.93 (d, J=11.1 Hz, 1H), 4.85 (d, J=11.1 Hz, 1H), 4.07 (q, J=7.2 Hz, 2H), 3.69 (s, 3H), 1.02 (t, J=7.2 Hz, 3H). 13C NMR: (100 MHz, CDCl3) delta 168.5, 159.7, 156.1, 148.6, 138.7, 132.1, 131.63, 131.56, 130.83, 130.80, 130.6, 129.93, 129.85, 129.64, 129.56, 129.2, 129.1, 128.1, 128.0, 127.3, 127.2, 110.2, 103.4, 70.2, 70.1, 60.8, 55.5, 14.0. IR: (film) 1721, 1503, 1289, 1251, 1020 cm?1. HRMS: (ESI+) m/z calc’d for (M+H)+ [C28H25NO5+H]+: 456.1805, found 456.1813. Diarylation product alcohol (6opdi): 1H NMR: (400 MHz, CDCl3) delta 7.90 (d, J=7.8 Hz, 2H), 7.57-7.49 (m, 2H), 7.46-7.38 (m, 4H), 7.22 (s, 2H), 4.69 (d, J=5.9 Hz, 2H), 4.17 (app. br. s, 4H), 3.01 (s, 3H), 1.66 (t, J=5.9 Hz, 1H), 1.12 (t, J=7.0 Hz, 6H). 13C NMR: (125 MHz, CDCl3) delta 168.2, 153.7, 139.0, 136.0, 135.2, 131.6, 131.3, 129.9, 128.6, 127.5, 65.2, 61.0, 60.1, 14.1. IR: (film) 3473, 1717, 1291, 1254, 1131 cm?1.HRMS: (ESI+) m/z calc’d for (M+Na)+ [C26H26O6+Na]+: 457.1622, found 457.1627.

According to the analysis of related databases, 1829-28-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; The University of Georgia Research Foundation, Inc; Ferreira, Eric; Li, Qiankun; (47 pag.)US2018/65909; (2018); 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. 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,4-Dibromo-2,5-diiodobenzene

100 ml to double-mouth bottle 1,4-dibromo -2,5- phenyl-diiodide 974.5 mg (2mmol), phenylboronic acid 609.5 mg (5mmol), four (triphenylphosphine) palladium 115.6 mg (0.1mmol), vacuum heat nitrogen three times post-injection by adding oxygen-free tetrahydrofuran 20 ml aqueous solution of potassium carbonate and the 10 ml (2mol/L), in 74 C lower reflux 8h, DCM extraction for reaction is ended, and salt water washing three phase after drying with anhydrous sodium sulfate, after filtration turns on lathe does, with pure petroleum ether column separation and purification, to obtain white powder 2,5-dibromo -1,4- diphenyl benzene, the yield is 63.7%, that is, the intermediate product 1. Product characterization data are as follows

The synthetic route of 63262-06-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University; Li, Lingzhi; Qin, Anjun; Tang, Benzhong; Sun, Jingzhi; (15 pag.)CN104844475; (2016); B;,
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 41252-98-6 as follows. Safety of 1-Iodo-2-methyl-3-nitrobenzene

Step 2 3-(2-Iodo-6-nitro-phenyl)-2-oxo-propionic acid Sodium ethoxide solution (35 ml, 44 mmol) in an ice-water bath was added dropwise with a solution of 1-iodo-2-methyl-3-nitro-benzene 74b in ethanol (35 ml, 40 mmol) under an argon atmosphere. Upon completion of the addition, the reaction mixture was stirred until lots of brown precipitates were formed, and added with diethyl oxalate (6 ml, 44 mmol) in one portion. The reaction mixture was refluxed at 100 C. in an oil bath for 0.5 hour, added with water (70 ml) and refluxed for another 1 hour. The reaction mixture was concentrated under reduced pressure to evaporate ethanol, washed with ethyl acetate (50 ml) under base condition, adjusted to pH 3 with hydrochloric acid (1M), and extracted with ethyl acetate (30 ml*3). The combined organic extracts were washed with saturated brine (30 ml), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to obtain the title compound 3-(2-iodo-6-nitro-phenyl)-2-oxo-propionic acid 74c (2.94 g) as a brown oil to be used directly in the next step.

According to the analysis of related databases, 41252-98-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ChoTang, Peng Cho; Su, Yidong; Li, Yali; Zhang, Lei; Zhao, Fuqiang; Yang, Jialiang; Zhou, Ying; Bie, Pingyan; Qian, Guangtao; Ju, Minggang; US2010/75952; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 7681-82-5, These common heterocyclic compound, 7681-82-5, name is Sodium iodide, 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 typical example is exemplified by the synthesis of 4b: To a stirred solution of TMEDA (1.36 mL,9 mmol) in hexane (5 mL) was added dropwise at ice bath temperature n-butyllithium (9 mmol) in hexane followed by acetophenone trimethylsilyl enol ether 1 (576 mg, 3 mmol), and the mixture was stirred for 24 h at room temperature. In a separate flask, a mixture of bismuth(III) chloride (315.5 mg,1 mmol) and tris(4-methylphenyl)bismuthane (964 mg, 2 mmol) was stirred in ether (10 mL) at room temperature for 1 h. To the suspension of chlorobis(4-methylphenyl)bismuthane (ca. 3 mmol) thus formed was added sodium iodide (450 mg, 3 mmol) and a few drops of 15-crown-5 ether and the resulting yellowish mixture was stirred for 3 h at room temperature. To a suspension of the lithium compound previously prepared was added at room temperature magnesium dibromide diethyl etherate (775 mg, 3 mmol) followed by, at -30 C, a suspension of iodobis(4-methylphenyl)bismuthane(ca. 9 mmol), and the resulting mixture was stirred for 1 h, during which time the temperature was raised to ambient temperature. The reaction mixture was poured into brine (50 mL) and extracted with ethyl acetate (50 mL × 3). The combined extracts were concentrated to leave an oily residue, which was purified by chromatography (silica gel) using hexane-ethyl acetate (5:1) as the eluent to afford 4b in 30% yield (459 mg, 0.9 mmol). Because 4a, 4f and 10 underwent decomposition when purified by chromatography on silica gel, these compounds were converted into the corresponding halobismuthanes 5a, 5f and 11, respectively, without isolation.

Statistics shows that Sodium iodide is playing an increasingly important role. we look forward to future research findings about 7681-82-5.

Reference:
Article; Murafuji, Toshihiro; Tomura, Mai; Ishiguro, Katsuya; Miyakawa, Isamu; Molecules; vol. 19; 8; (2014); p. 11077 – 11095;,
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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C7H4F3I

Into a 20-mL microwave tube purged and maintained with an inert atmosphere of nitrogen, was placed a solution of methyl 2′-oxo-3,4-dihydro-lH-spiro[naphthalene-2,3′- pyrrolidine]-8-carboxylate (100 mg, 0.39 mmol, 1 equiv) in toluene (5 mL), l-iodo-2- (trifluoromethyl)benzene (210 mg, 0.77 mmol, 2 equiv), Cul (7 mg, 0.04 mmol, 0.1 equiv), methyl[2-(methylamino)ethyl]amine (7 mg, 0.08 mmol, 0.2 equiv) and K3PO4 (250 mg, 1.18 mmol, 3 equiv). The resulting solution was stirred overnight at 110 °C. The reaction mixture was cooled to room temperature and then poured into 20 mL of water. The resulting solution was extracted with 3×20 mL of EtOAc. The combined organic layers were dried over anhydrous Na2SC”4, filtered, and concentrated under vacuum. The residue was purified by preparative TLC with EtO Ac/petroleum ether (1 :3). The collected fractions were concentrated under vacuum to give 50 mg (32percent yield) of the title compound as yellow oil. MS: (ES, m/z): 404 [M+H]+.

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FORMA THERAPEUTICS, INC.; H. LEE MOFFITT CANCER CENTER AND RESEARCH INSTITUTE, INC.; LEE, Jennifer; BURNETTE, Pearlie; CHELLAPPAN, Srikumar; BARCZAK, Nicholas; CONTI, Chiara; ESCOBEDO, Jaime A.; HAN, Bingsong; LANCIA, David R., Jr.; LIU, Cuixian; MARTIN, Matthew W.; NG, Pui Yee; RUDNITSKAYA, Aleksandra; THOMASON, Jennifer R.; ZHENG, Xiaozhang; (322 pag.)WO2018/75959; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 455-13-0,Some common heterocyclic compound, 455-13-0, name is 4-Iodobenzotrifluoride, molecular formula is C7H4F3I, 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: In a flame-driedvessel, equipped with a magnetic stirrer, under argon atmosphere,were added 0.3 mL of anhydrous acetonitrile, the nucleophile (imidazoleor benzimidazole – 0.75 mmol, 1.5 eq.), the electrophile(alkyl or aryl iodide – 0.5 mmol, 1 eq.), the base (1 mmol, 2 eq.),and the copper catalyst (0.05 mmol – 10% loading). The reactionvessel was heated to 80 C and left under stirring for 24 h. Thereaction mixture was then allowed to cool to room temperature,diluted with dichloromethane (5 mL) and filtered through celite. The celitepad was further washed with dichloromethane(2 x 5 mL). The combined organic phases were washed with water(2 x 5 mL) and brine (2 x 5 mL). The organic solvents were thenremoved in vacuo to yield the crude product, which was purifiedby flash column chromatography on silica gel using a gradient mixtureof ethyl acetate/petroleum ether as eluent. The 1H and 13CNMR spectral data for all N-arylatedimidazoles and benzimidazolesare in full agreement with those reported to literature [57-61].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Iodobenzotrifluoride, its application will become more common.

Reference:
Article; Milenkovi?, Milica R.; Papastavrou, Argyro T.; Radanovi?, Du?anka; Pevec, Andrej; Jagli?i?, Zvonko; Zlatar, Matija; Gruden, Maja; Vougioukalakis, Georgios C.; Turel, Iztok; An?elkovi?, Katarina; ?obelji?, Bo?idar; Polyhedron; vol. 165; (2019); p. 22 – 30;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com