Tag: M.W=200-300

Adding a certain compound to certain chemical reactions, such as: 202865-85-8, name is 1-Bromo-4-iodo-2-methylbenzene, 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 202865-85-8, COA of Formula: C7H6BrI

Under an argon atmosphere, Intermediate 6 (1.20 g, 2.40 mmol),1-Bromo-4-iodo-2-methylbenzene (Intermediate 11) (852 mg, 2.88 mmol)(1.68 g, 4.80 mmol, manufactured by Wako Pure Chemical Industries, Ltd.) and copper iodide (91.4 mg, 0.48 mmol, 0.35 mmol) were added to a solution of L-proline (110 mg, 0.96 mmol; manufactured by Wako Pure Chemical Industries, : Manufactured by Wako Pure Chemical Industries, Ltd.) Dimethylformamide (2.4 ml, manufactured by Wako Pure Chemical Industries, Ltd.) was stirred under an argon atmosphere for 48 hours, At 110 CAnd heated.Next, after cooling to room temperature, a saturated aqueous solution of ammonium chloride (30 ml) and dichloromethane (100 ml) were added to the reaction mixture, followed by liquid separation. The organic layer was dried over magnesium sulfate and the residue was purified by silica gel column chromatography (dichloromethane 20%, hexane 80%) to obtain Intermediate 12 as pale yellow crystals (1.43 g, yield 89%)

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Reference:
Patent; Kokuritsu Daigaku Hojin Kyushu Daigaku; Kaji, Hironori; Suzuki, Hajime; Suzuki, Katsuaki; Oheiwa, Hajime; Wakamiya, Atsushi; Fukushima, Tatsuya; Suzuki, Huritz; Murata, Yaseujiro; Sieje, Kacheuyuki; Adachi, Jihaya; (48 pag.)KR2015/123907; (2015); 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. 18698-96-9, name is 2-(2-Iodophenyl)acetic acid, A new synthetic method of this compound is introduced below., Recommanded Product: 2-(2-Iodophenyl)acetic acid

General procedure: A 50 mL, round-bottom flask equipped with a magnetic stir bar was charged with carboxylic acid (2 equiv), HOBT (2 equiv) and EDCI (2 equiv). The reagents were dissolved in DCM and the solution was allowed to stir for 15 min. Subsequently, different amino compounds (11-13) (1 equiv) and TEA (5 equiv) were added to the reaction vessel and the solution was allowed to react at 25 °C for 8 h. Upon completion, the solvent was removed under reduced pressure and the residue was purified by flash chromatography (SiO2, DCM: MeOH = 20:1) to afford corresponding compounds 14a-14k.

The synthetic route of 18698-96-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tang, Le; Ren, Jing; Ma, Yuchi; Wang, Xin; Chen, Lin; Shen, Jingkang; Chen, Yue-Lei; Xiong, Bing; Tetrahedron Letters; vol. 57; 21; (2016); p. 2311 – 2314;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, 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 5876-51-7, category: iodides-buliding-blocks

[00228] To 26.1 mg PdCl2(dppf).CH2Cl2 in a reaction tube under nitrogen were added 4 ml dioxane, 0.12 ml (1.0 mmol) of N-methypiperidine, 0.16 ml (1.1 mmol) pinacolborane and 253 mg (1.02 mmol) 1-iodo-3,4-methylenedioxybenzene. The red reaction solution was warmed to 80 C. with stirring for 17 h in an oil bath. Analysis of the dark green reaction solution by gc as described above gave the reaction product distribution: 1,3-benzodioxole (16% of gc peak area); the pinacol ester of phenylboronic acid (7%) and the desired arylboronic acid pinacol ester (peak area 76%). Increasing the N-methypiperidine concentration to 3 mmol had little effect on product distribution. Found: 1,3-benzodioxole (17% of gc peak area); the pinacol ester of phenylboronic acid (8%) and the pinacol ester of 3,4-methylenedioxyphenylboronic acid (peak area 75%).

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, 5-Iodobenzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Commonwealth Scientific and Industrial Research Organisation; US6680401; (2004); B1;,
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. 13329-40-3, name is 1-(4-Iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1-(4-Iodophenyl)ethanone

To a clear dark solution of l-(4-iodophenyl)ethanone (1.046 kg, 4.251 mol, 1 equiv.) in DCM (8 L) was charged (dropwise) bromine (228 ml, 4.45 mol, 1.047 equiv.) over the period of 30 to 45 min at the ambient temperature. The reaction was slightly exothermic (temperature incresed to about 20-25 C) and released a lot of hydrogen bromide gas as the by-product. The reaction was considered as complete after 3 to 4 hrs as indicated by HPLC (typically ~7% starting material, -10% di-bromo by- product, and ~83%> desired mono-bromo product, all in area%> by HPLC). It was then quenched and neutralized by aqueous NaHC03solution wash (4 L), followed by brine wash (3 L). Upon drying over Na2S04, it is rotavapped and solvent swapped to THF and the desired product was crystallized from THF (final volume about 2 L) at from 50C to 20C to afford the 1st crop: 340 g (98% HPLC purity); by concentrating the mother liqor to about half-volume to afford the 2nd crop: 426 g (98%o HPLC purity); by further concentating and addition of hexanes (i.e.,THF/hexanes, 1 : 1) to afford the 3rd crop: 339 g (97+% HPLC purity). The combined crystal title compound was 1.105 kg (80% yield). 1H NMR (500 MHz, CDC13): 7.88 (d, 2 H), 7.70 (d, 2 H), 4.42 (s, 2 H).

According to the analysis of related databases, 13329-40-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ENANTA PHARMACEUTICALS, INC.; TANG, Datong; XU, Guoyou; PENG, Xiaowen; YING, Lu; WANG, Ce; CAO, Hui; LONG, Jiang; KIM, In, Jong; WANG, Guoqiang; QIU, Yao-ling; OR, Yat, Sun; WO2013/59281; (2013); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4387-36-4, A common heterocyclic compound, 4387-36-4, name is 2-Iodobenzonitrile, molecular formula is C7H4IN, 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: An oven dried two-necked round bottom flask was charged with aryl halide (1mmol) and K3PO4 (2mmol), evacuated and backfilled with argon. The azole compound (1mmol) and 2mL of DMSO were added under argon. After that Cu-NP (1.6mmol) was added and the flask was again backfilled with argon. The flask was then immersed in a preheated oil bath at 80°C until the conversion was completed (detected by TLC). The cooled mixture was partitioned between ethyl acetate (10mL) and saturated NH4Cl (10mL). The aqueous layer was extracted with ethyl acetate (2×10mL), the organic layer was washed with brine (20mL), dried over anhydrous Na2SO4 and concentrated in vacuum. The residue was purified by column chromatography on silica gel using ethyl acetate in hexane (1.5?10percent) as eluent to afford the desired product. All the products have been characterized by 1H NMR, 13C NMR, and mass spectroscopy. For new products, FTIR data were also recorded.

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:
Article; Pai, Gita; Chattopadhyay, Asoke P.; Tetrahedron Letters; vol. 57; 29; (2016); p. 3140 – 3145;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 6940-76-7, 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 6940-76-7 as follows.

EXAMPLE 14; Ethyl 4-(3-chloropropyl)-4-cyano-1-piperidinecarboxylate; To a solution of ethyl 4-cyano-1-piperidinecarboxylate (6.0 g) in tetrahydrofuran (120 ml) at -70C, under nitrogen, was added a solution of lithium diisopropylamide (4.6 g) in tetrahydrofuran (21.5 ml), dropwise, with stirring. The reaction was allowed to warm to -10C and after 30 min was recooled to -70C. A solution of 1-chloro-3-iodopropane (7.4 g) in tetrahydrofuran (20 ml) was added to the mixture over 30 min. The reaction mixture was quenched with water and allowed to warm to ambient temperature. The mixture was extracted with ethyl acetate. The extracts were washed with water, saturated sodium chloride solution, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentratedin vacuo and the residue was flash chromatographed (silica), eluting with 2:1 heptane/ethyl acetate. The appropriate fractions were collected and concentrated to afford 5.5 g (64%) of product; Calculated for C12H19ClN2O2 ; 55.70%C; 7.40%H; 10.83%N; Found; 55.88%C; 7.67%H; 10.80%N

According to the analysis of related databases, 6940-76-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Aventis Pharmaceuticals Inc.; EP892802; (2003); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 610-97-9, A common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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: General procedure carbonylative cyclization ofmethyl-2-iodobenoate/1,2-diiodo benzene for the synthesis ofN-substituted isoindole-1,3-diones using ImmPd-IL as a catalystIn a 100 mL stainless steel autoclave, methyl-2-iodobenoate/1,2-diiodobenzene (1 mmol), aryl amine (2 mmol), ImmPd-IL(2 mol%), toluene (10 mL) and Et3N (2.5 mmol) were added. Theautoclave was closed, purged three times with nitrogen followedwith carbon monoxide, and then pressurized with 1 atm of CO andheated at 100C for 6 h. After completion of reaction the reac-tor was cooled to room temperature, the remaining CO gas wascarefully vented, and the reactor was opened. The reactor vesselwas thoroughly washed with ethyl acetate (10-15 mL) to removeany traces of product and catalyst if present. The catalyst was fil-tered and the reaction mixture was evaporated under vacuum. Theresidue obtained was purified by column chromatography (silicagel, 60-120 mesh; petroleum ether/ethyl acetate, 95:05) to affordthe desired product. The products were confirmed by GC, GC-MS,1H NMR and13C NMR spectroscopic techniques. The purity of com-pounds was determined by GC-MS analysis.

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:
Article; Khedkar, Mayur V.; Shinde, Ajinkya R.; Sasaki, Takehiko; Bhanage, Bhalchandra M.; Journal of Molecular Catalysis A: Chemical; vol. 385; (2014); p. 91 – 97;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 103962-05-6, 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 103962-05-6 as follows.

EXAMPLE 11; Step 1; To a solution of 4-(trifluoromethoxy)iodobenzene (0.54 mL, 3.45 mmol), 4-methoxyphenol (0.28 g, 2.26 mmol) and cesium carbonate (1.54 g, 4.73 mmol) in dioxane (10 mL) was added N,N-dimethylglycine hydrochloride (0.03 g, 0.22 mmol). The vessel was purged with nitrogen before Cu(I) iodide (0.02 g, 0.08 mmol) was added. The brownish-green reaction mixture was heated to 90° C. overnight. The reaction mixture was diluted with water and ethyl acetate. The organic portion was washed with brine, dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound (0.8 g, 100percent) as brown oil.

According to the analysis of related databases, 103962-05-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DECODE CHEMISTRY, INC.; US2007/66820; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 6940-76-7, name is 1-Chloro-3-iodopropane, 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 6940-76-7, COA of Formula: C3H6ClI

To a suspension of NaH (1.10 g, 60 % in mineral oil, 27.5 mmol) in THF (40 mL) at 0 was added a solution of triethyl phosphonoacetate (6.05 g, 5.3 mL, 27.0 mmol) in THF (20 mL) during a period of 5 min. The mixture was kept at 0 for 60 min. Then a solution of 1-chloro-3-iodopropane (2.04 g, 1.05 mL, 10.0 mmol) in THF (20 mL) was added dropwise over a period of 5 min. Then the mixture was kept at room temperature for an additional 24 h. The reaction was quenched by addition of saturated NH4Cl (15 mL), then THF was removed by vacuum distillation. The aqueous phase was extracted with EtOAc (30 mL*3), and washed with brine (40 mL). The combined organic layers were dried over NaSO4 and concentrated. The residue was purified by flash chromatography to give the substitued phosphonoacetate 6 (rotamers in a 1:1 ratio) as a slight yellow oil (2.54 g, 84% yield from the 1-chloro-3-iodopropane 8).

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-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yi, Ming; Gu, Peiming; Kang, Xiao-Yan; Sun, Jian; Li, Rui; Li, Xue-Qiang; Tetrahedron Letters; vol. 55; 1; (2014); p. 105 – 107;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 83863-33-6,Some common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-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.

To a solution of 5-iodo-2-methyl-phenylamine (0.5 g, 1.62 mmol) (Aldrich) in toluene (5 mL) were added 2-(tri-n-butylstannyl-oxazole (0.5 mL, 2.43 mmol) (Aldrich) and tetrakis-(triphenyl-phosphine)palladium(0) (0.018 g, 0.01 mmol) (Strem Chemicals). The reaction mixture was heated at 100 C. for 14 hours. The reaction mixture was cooled down and the solvent was evaporated. The crude material was then purified by column chromatography. The desired product was eluted with 40% EtOAc. The desired fractions were evaporated to afford 2-methyl-5-oxazol-2-yl-phenylamine. (Yield 0.03 g, 11%). HR-MS (ES+) m/z Calculated for C10H11N2O ([M+H]+): 175.0866. Found: 175.0865.

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

Reference:
Patent; Dominique, Romyr; Luk, Kin-Chun; Qiao, Qi; Rossman, Pamela Loreen; US2012/184548; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com