Iodides-buliding-blocks

914225-70-0,Some common heterocyclic compound, 914225-70-0, name is 1-(5-Fluoro-2-iodophenyl)ethanone, molecular formula is C8H6FIO, 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.

Preparation 1051-(2-Acetyl-4-fl ro-phenyl)-pyrrolidin-2-one1 ,4-Dioxane (50 ml_) was degassed by heating briefly to reflux and bubbling nitrogen gas through the solvent for 10 minutes, whilst it cooled to room temperature. Cul (180 mg, 5 mol%), glycine (284 mg, 20 mol%), 2-pyrrolidinone (1.73ml_, 22.73 mmol), K3PO4 (10.05 g, 47.35 mmol) and 1-(5-fluoro-2-iodo-phenyl)-ethanone (5.0 g, 18.94 mmol) were added sequentially to the solvent and the reaction mixture was heated at 100C under N2 for 10 hours. The reaction mixture was filtered through a celite plug, eluting with EtOAc and the filtrate was concentrated. The crude product was purified by flash chromatography (5% MeOH in DCM) to give the title compound (2.02 g, 48% yield) as a yellow oil1H NMR (400 MHz, CDCI3): delta ppm 2.20 (2H, pentet), 2.47 (2H, t), 2.54 (3H, s), 3.83 (2H, t), 7.17-7.21 (2H ,m), 7.28-7.32 (1 H, m). MS:: m/z 222 [MH]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(5-Fluoro-2-iodophenyl)ethanone, its application will become more common.

Reference:
Patent; PFIZER INC.; BUNNAGE, Mark, Edward; COOK, Andrew, Simon; CUI, Jingrong, Jean; DACK, Kevin, Neil; DEAL, Judith, Gail; GU, Danlin; HE, Mingying; JOHNSON, Patrick, Stephen; JOHNSON, Ted, William; LE, Phuong, Thi, Quy; PALMER, Cynthia, Louise; SHEN, Hong; WO2011/138751; (2011); A2;,
Iodide – Wikipedia,
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The chemical industry reduces the impact on the environment during synthesis 6293-83-0, name is 2-Iodo-4-nitroaniline, I believe this compound will play a more active role in future production and life. 6293-83-0

Example 6 (examples of the reaction formula (3)) [of 18] To a 2-iodo-4-nitroaniline 12 (7. 50 g, 28. 4 mmol), bis(triphenylphosphine)palladium dichloride (99. 6mg,0 ? 142 mmol) and copper(I) iodide (54. 1 mg, 0. 284 mmol) in ethyl acetate (49. 9 mL) solution at room temperature, the diethylamine (10. 4 g, 142 mmol) and the terminal acetylene 11 (11. 5g, 42. 6 mmol) in toluene (28.9mL) was added. Furthermore, the reaction mixture was heated to 50 C, and stirred for 6 hours. To the resulting reaction mixed solution is added with activated carbon (0.750g), in 50 C is filtered to remove the activated carbon and the reaction residue, adding water in the filtrate (22.5 ml), separating the organic phase. Furthermore, the solvent of the organic phase the distill goes under reduced pressure, the crude product obtained by adding toluene (46.2 ml), activated carbon (1.15g), in not more than 80 C lower filtering to remove the temperature of the activated carbon, the target is obtained by re-crystallization from filtrate nitryl body 13 (10.3g, 25.2 mmol, yield 89%). Nitro compound 13 through the structure of1H-NMR analysis identified, with the above-mentioned embodiment of the results of 5 the nitro compound obtained in 13 the1H-NMR completely identical.

The chemical industry reduces the impact on the environment during synthesis 6293-83-0. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Nissan Chemical Industries, Ltd.; Takayama, Yuki; Nagao, Masato; (20 pag.)CN103068795; (2016); B;,
Iodide – Wikipedia,
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1878-69-9,Some common heterocyclic compound, 1878-69-9, name is 2-(3-Iodophenyl)acetic acid, molecular formula is C8H7IO2, 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.

In a 100 mL hydrothermal synthesis reactor, sodium hydroxide (3 mmol) and water (5 mL) were added.After stirring and stirring, m-iodophenylacetic acid (0.5 mmol) and cuprous oxide (0.05 mmol) were added.White lignan (0.05 mmol), the reaction was stirred at 100 C for 6 hours.After cooling, the pH was adjusted to 2 with dilute hydrochloric acid and extracted with ethyl acetate.The extract is concentrated and subjected to column chromatography to obtain m-hydroxyphenylacetic acid.54.0 mg, yield 71%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(3-Iodophenyl)acetic acid, its application will become more common.

Reference:
Patent; Shenyang Pharmaceutical University; Yunnan Tropical Crop Science Institute; Chen Guoliang; Wu Ying; Bao Xuefei; Li Guohua; Liang Xinjie; Jiang Shikuan; Zhou Qifan; Du Fangyu; (11 pag.)CN109970542; (2019); A;,
Iodide – Wikipedia,
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74-88-4, A common heterocyclic compound, 74-88-4, name is Iodomethane, molecular formula is CH3I, 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.

Preparation of 7-ethoxy-4-(3-iodo-4,5-dimethoxybenzyl)isoquinolin-8-ol hydrochloride 723-lodo-4,5-dimethoxybenzaldehvde RBO 40110In a 100 mL round bottom flask 3-iodo-4-hydroxy-5-methoxybenzaldehyde (1 .0 g, 3.60 mmol) was dissolved in acetone (50 mL) and K2CO3 (746 mg, 5.40 mmol) was added at RT. The reaction mixture was stirred at RT for 30 min, then iodomethane (766 mg, 5.40 mmol) was added and reaction was stirred at reflux for another 4 h. Acetone was removed and the residue was taken back in EtOAc (50 mL) and H2O (50 ml_). The aqueous layer was further extracted with EtOAc (3×50 ml_). The combined rganics layers were washed with brine (50 ml_), dried over Na2SO4, filtered and concentrated to dryness to give 3-iodo-4,5-dimethoxybenzaldehyde RBO 40110 (603 mg, 57% yield) as a brown oil.RBO 40110MW: 292.07; Yield: 57%; Brown oil.1H-NMR (CDCIs, delta): 3.93 (s, 6H, 2xOMe), 7.41 (s, 1 H, ArH), 7.84 (s, 1 H, ArH), 9.82 (s, 1 H, CHO).MS-ESI m/z (% rel. Int.): 293 ([MH]+, 100).HPLC: Method A, XBridge column, detection UV 254 nm, RT = 5.53 min, peak area 97.0%.

The synthetic route of 74-88-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EXONHIT S.A.; LEBLOND, Bertrand; TAVERNE, Thierry; BEAUSOLEIL, Eric; CHAUVIGNAC, Cedric; CASAGRANDE, Anne-Sophie; DESIRE, Laurent; WO2011/151423; (2011); A1;,
Iodide – Wikipedia,
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672-57-1, Adding a certain compound to certain chemical reactions, such as: 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, 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 672-57-1.

General procedure: To an oven-dry ground test tube equipped with a stir bar were added 1 mmol 2-bromoiodobenzene, 1mmolL-alaninamide, 3 mmol potassium carbonate and 5 mL DMF. The test tube was sealed with a rubber stopperand was evacuated and refilled with argon for three times. Then the test tube was stirred in an oil bathpreheated at 90? C for 48 hours. After the test tube was cooled to room temperature, the reaction wasquenched with water, and the reaction mixture was extracted with 20 mL ethyl acetate for three times. Thecombined organic layer was washed with 10 mL water and then saturated sodium chloride aqueous solution,and dried over anhydrous sodium sulfate. After filtration, the filtrate was condensed on a rotary evaporator invacuum. The resulting crude product was chromatographed on silica gel (300-400 mesh) with a 1:2 volumeratio mixed solution of ethyl acetate and petroleum ether as eluent to give a white solid L-N-phenylalaninamide.

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-Chloro-2-iodo-4-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wang, Yan; Tu, Xingzhao; Lv, Xirui; Zhou, Lihong; Zeng, Qingle; Tetrahedron Letters; vol. 54; 45; (2013); p. 6045 – 6048;,
Iodide – Wikipedia,
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A common compound: 39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 39998-81-7

2-fluoro-4-iodotoluene 25g (105.9mmol, 1.0eq), AIBN 417mg (2.5mmol, 0.024eq),Co(OAc)2¡¤4H2O 1.3g (7.3mmol, 0.049eq), NaBr 360mg (4.9mmol, 0.033eq), dissolved in HOAc 250mL (10V), stirred for total use,The temperature of the outer bath of the reaction coil was raised to 130 C, and the coil pressure was adjusted to 1.2 MPa with oxygen to start the charging. The residence time of the system was 1.5 h and the oxygen was 3 to 5 eq.The system was directly pumped into 375 mL of purified water, and the pH of the system was adjusted to 12-14 with NaOH solids.The aqueous phase was extracted twice with 125 mL MTBE, and the aqueous phase was adjusted to pH 1 with concentrated HCl.A large amount of solid was precipitated, and 9.9 g of the target product was obtained by filtration, and the yield was 35%.

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, 39998-81-7, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jilinkai Laiying Pharmaceutical And Chemical Co., Ltd.; Hong Hao; Zhang Enxuan; Lu Jiangping; Liu Zhiqing; Li Chao; Tan Yang; (16 pag.)CN110218150; (2019); A;,
Iodide – Wikipedia,
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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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, A new synthetic method of this compound is introduced below., 3032-81-3

1,3-Dichloro-5-iodobenzene (2.73 g, 10 mmol) was added to the reaction flask under an argon atmosphere.3,5-dichlorothiophenol (2.15 g, 12 mmol), cuprous iodide (9.5 mg, 0.5 mmol),Potassium carbonate (6.9 g, 50 mmol) and 50 ml of DMF solvent were stirred and heated to 120 ¡ã C for 12 h.After the reaction was stopped, the solvent was evaporated to dryness and extracted with dichloromethane.Purified by silica gel column chromatography, petroleum ether / dichloromethane mixed solvent (15 / 1, v / v) as a rinse to give a white solid, yield 75percent;

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; South China Xietong Chuangxin Institute; Ying Lei; Hu Liwen; Huang Fei; Cao Yong; (25 pag.)CN109096159; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

135050-44-1, A common compound: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

2-Ethynylpyridine (0.57 mL, 5.6 mmol), 4-iodo-3-chloroaniline (1.01 g, 4.0 mmol), PdCl2(PPh3)2 (281 mg, 0.4 mmol), copper (I) iodide (152 mg, 0.8 mmol), trimethylamine (5.6 mL, 40 mmol) and DMF (4.5 mL) were added to a vial with a stirbar and the mixture was sparged with Argon. The reaction mixture was heated in a 90 C heating block for 45 min then cooled to ambient temperature. The mixture was partitioned between water and ethyl acetate, and the organic layer was washed with brine, dried over Na2S04, filtered and evaporated under reduced pressure. The crude product was purified by gradient flash column chromatography from 0 – 100% EtOAc in hexanes to yield 660 mg (72%) of 3-chloro-4-(pyridin-2-ylethynyl)aniline (12) as a yellow solid. 1H MR (400 MHz, CDC13) delta 8.61 (s, 1H), 7.69 (t, J= 7.7 Hz, 1H), 7.54 (d, J= 7.8 Hz, 1H), 7.41 (d, J= 8.4 Hz, 1H), 7.26 – 7.21 (m, 1H), 6.72 (s, 1H), 6.53 (d, J= 8.4 Hz, 1H), 3.95 (br s, 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, 3-Chloro-4-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE CALIFORNIA INSTITUTE FOR BIOMEDICAL RESEARCH; UNIVERSITAeT BREMEN; PETRASSI, Hank Michael James; PERAM SURAKATTULA, Murali Mohan Reddy; MAEDLER, Kathrin; ARDESTANI, Amin; ROLAND, Jason T.; BAGULEY, Tyler D.; TREMBLAY, Matthew S.; SHEN, Weijun; SCHULTZ, Peter G.; CHATTERJEE, Arnab K.; (155 pag.)WO2016/210345; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

455-13-0, 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. 455-13-0 name is 4-Iodobenzotrifluoride, 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.

General procedure: A 25-mL flask was charged with Pd(OAc)2 (1.2 mg, 0.005 mmol), 1-iodo-4-nitrobenzene (1a, 127.0 mg, 0.5 mmol), K2CO3 (141.0 mg, 1.0 mmol), H2O (0.5 mL), and PEG 400 (2.0 mL); the flask was subjected to standard cycles (3 ¡Á) of evacuation and back-filling with dry and pure CO. The mixture was stirred at r.t. for the indicated time. The mixture was poured into sat. aq NaCl (15 mL), acidified to pH 3 with 3 M aq HCl, and extracted with EtOAc (3 ¡Á 15 mL). The solvent was removed from the combined organic phases on a rotary evaporator. The crude product was purified by column chromatography (silica gel, PE-EtOAc-HCO2H, 25:1:1) to afford 2a as a light yellow solid; yield: 75mg (90%); mp 238.0-239.3 C. 1H NMR (400 MHz, DMSO-d6): delta = 13.68 (br s, 1 H), 8.30 (d, J = 8.0 Hz,2 H), 8.14 (d, J = 8.0 Hz, 2 H). 13C NMR (100 MHz, DMSO-d6): delta = 165.9, 150.0, 136.4, 130.7, 123.8.

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

Reference:
Article; Han, Wei; Jin, Fengli; Zhou, Qing; Synthesis; vol. 47; 13; (2015); p. 1861 – 1868;,
Iodide – Wikipedia,
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64248-58-4, A common compound: 64248-58-4, name is 1,2-Difluoro-4-iodobenzene, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

Example 40; 4- {6-[2-(3,4-Difluorophenyl)-l -ethynyl]-3-pyridazinyl}piperazino-2(trifluoromethyl)- phenylmethanone; Prepared by Sonogashira coupling reaction of Intermediate 6 with l,2-difluoro-4- iodobenzene in a mixture of triethylamine and DMSO to give the product as a white solid; IR (KBr) 2856, 2220, 1655, 1510, 1265, 1147, 1009 cm”1; 1H NMR (300 MHz, CDCl3) delta 3.32- 3.36 (m, 2H), 3.72-4.10 (m, 6H), 6.88 (d, J= 9.3 Hz, IH), 7.12-7.16 (m IH), 7.28-7.65 (m, 6H), 7.73 (d, J= 9.3 Hz, IH) ; ESI-MS (m/z) 472.62 (M)+.

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, 1,2-Difluoro-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; WO2008/62276; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com