Category: iodides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, 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 5471-81-8, category: iodides-buliding-blocks

Under a protective atmosphere of inert gas, Pd(OAc)2 (2.2 mg, 10 mol%), XPhos (19.1 mg, 20 mol%), NBE-CO2K (3.5 mg, were added to a 4.0 mL reaction flask equipped with a magnetic stir bar. 10mol%),Methyl 3-methyl-4-iodobenzoate (0.2 mmol, 1.0 equiv.),Glycidyl butyrate (0.6 mmol, 3.0 equiv.)And dry N-methylpyrrolidone (1.0 mL).The reaction flask was capped and stirred at room temperature for about 5 minutes.The mixture was then heated to 80 C and stirred for 24 hours. After the reaction mixture was cooled to EtOAc EtOAc EtOAc m. Purified by column chromatography, the eluent was petroleum ether: ethyl acetate = 10:1 (v/v),53 mg of methyl 7-methyl-2-(butyryloxymethyl)-2,3-dihydrobenzofuran-5-carboxylate (light yellow oily liquid, yield 91%)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 4-iodo-3-methylbenzoate, and friends who are interested can also refer to it.

Reference:
Patent; Wuhan University; Zhou Qianghui; Wu Chenggui; Cheng Honggang; (20 pag.)CN108329285; (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. 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 620621-48-9

Intermediate 71 : methyl 2-chloro-5-(4-(dimethylamino)piperidin-l-yl)benzoate; Methyl 2-chloro-5-iodobenzoate (1.0Og, 3.37 mmol), cesium carbonate (0.360 mL,4.50 mmol), BINAP (0.070 g, 0.11 mmol), palladium(II) acetate (0.025 g, 0.11 mmol) and 4-(dimethylamino)piperidine (0.519 g, 4.05 mmol) were suspended in dioxane (18 mL) and sealed into a microwave tube. The reaction was heated to 120 0C for 3 hours in the microwave reactor and cooled to RT. The reaction mixture was filtered through celite. The crude product was purified by flash silica chromatography, elution gradient 0 to 10%NHVMeOH in DCM. Pure fractions were evaporated to dryness to afford methyl 2-chloro- 5-(4-(dimethylamino)piperidin-l-yl)benzoate (0.456 g, 68.3 %) as a yellow oil. m/z (ESI+) (M+H)+ =297.45; HPLC tR = 1.01 min. 1H NMR (400.13 MHz, CDC13) delta 1.56 – 1.66 (2H, m), 1.93 (2H, d), 2.24 – 2.29 (IH, m), 2.31 (6H, s), 2.71 – 2.78 (2H, m), 3.71 (2H, d), 3.92 (3H, s), 6.94 – 6.97 (IH, m), 7.27 – 7.28 (IH, m), 7.33 (IH, d).

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; AstraZeneca AB; AstraZeneca UK Limited; WO2009/47558; (2009); 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. 624-75-9, name is 2-Iodoacetonitrile, A new synthetic method of this compound is introduced below., Formula: C2H2IN

A 500-mL three-neck round-bottomed flask equipped with an addition funnel, thermometer and charged with 118a (6.70 g, 37.4 mmol), Iodoacetonitrile (12.5 g, 74.9 mmol), iron (II) sulfate heptahydrate (5.20 g, 18.7 mmol) and dimethyl sulfoxide (250 mL). Hydrogen peroxide (35%, 18.2 g, 187 mmol) was added dropwise to the mixture in 1 h through a syringe pump at room temperature using a water bath. Iron (II) sulfateheptahydrate (2 to 3 equivalent) was added to the reaction mixture in portions to keep the temperature between 25 C to 35 C, until the color of the reaction mixture is deep red. If TLC show the reaction not completed, then more hydrogen peroxide (2-3 equivalent) and more iron (II) sulfate heptahydrate (1-2 equivalent) were added in the same manner until the reaction is completed. After that time, the reaction mixture was partitioned between saturated sodium bicarbonate solution (200 mL) and ethyl acetate (400 mL). The organic layer was separated, and the aqueous layer was extracted with ethyl acetate (2 x 100 mL). The combined organic layers were washed with saturated Sodium thiosulfate solution (50 mL), dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography to afford a 78% yield (6.40 g) of 118b as a yellow oil: ]H NMR (500 MHz, CDC13) delta 6.23 (s, 1H), 4.23 (s, 2H), 3.94 (t, 2H, J = 6.5 Hz), 3.81 (s, 3H), 2.74 (t, 2H, J = 6.5 Hz), 2.00 (m, 2H), 1.83 (m, 2H); (APCI+) m/z 219.3 (M+H)

The synthetic route of 624-75-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GILEAD CONNECTICUT, INC.; GENENTECH, INC.; BARBOSA, Antonio, J., M.; BLOMGREN, Peter, A.; CURRIE, Kevin, S.; KRISHNAMOORTHY, Ravi; KROPF, Jeffrey, E.; LEE, Seung H.; MITCHELL, Scott A.; ORTWINE, Daniel; SCHMITT, Aaron, C.; WANG, Xiaojing; XU, Jianjun; YOUNG, Wendy; ZHANG, Honglu; ZHAO, Zhongdong; ZHICHKIN, Pavel E.; WO2011/140488; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 170112-66-0, The chemical industry reduces the impact on the environment during synthesis 170112-66-0, name is 3,4,5-Trifluoroiodobenzene, I believe this compound will play a more active role in future production and life.

(S) -2- (1 ,3-Dioxoisoindolin-2-yl) -Itf-methoxy- 3- (3 , 4 , 5-trifluorophenyl) ropanamide (28s) The starting material 25 (10.0 mmol, 2.48 g) , Pd(OAc)2 (1.50 mmol, 337 mg) , and AgOAc (20.0 mmol, 3.34 g) were weighed in air and placed in a sealed tube (350 mL) with a magnetic stir bar. To the reaction mixture, aryl iodide (15 mmol), 2,6- lutidine (3.00 mmol, 0.3 mL) , and HFIP (100 mL) were added. The reaction mixture was first stirred at room temperature for 10 minutes and then heated to 90 C for 36 hours under vigorous stirring. Upon completion, the reaction mixture was cooled to room temperature, and HFIP was recovered by distillation. The residue was filtered with DCM and concentrated as crude product 28s.

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, 3,4,5-Trifluoroiodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE SCRIPPS RESEARCH INSTITUTE; YU, Jin-Quan; WO2015/131100; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, 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 82998-57-0, Quality Control of 3-Iodo-4-methylbenzoic acid

Compound 5.3. Methyl 3-iodo-4-methylbenzoate. To a solution of 3-iodo-4- methylbenzoic acid (28.0 g, 0.107 mol) in MeOH (300 mL) at 0 C was carefully added concentrated H2SO4 (30 mL). The mixture was heated at 60 C overnight, then cooled and the solvent removed under reduced pressure. The residue was carefully poured onto ice- water (200 mL) and the mixture was extracted with EtOAc (500 mL). The organics was washed with water (100 mL), saturated NaHC03 (100 mL), brine (100 mL), dried (MgS04), filtered, and concentrated to yield the title compound as a brown oi 1 (29.0 g, 98%). ‘H NMR (400 MHz, CDCI3) delta 8.47 (d, J = 1 .7 Hz, 1 H), 7.90 (dd, J = 7.9 Hz, 1.7 Hz, 1 H), 7.29 (d, J= 7.9 Hz , 1 H), 3.90 (s, 2H), 2.48 (s, 3H).

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-Iodo-4-methylbenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; 3-V BIOSCIENCES, INC.; OSLOB, Johan D.; MCDOWELL, Robert S.; JOHNSON, Russell; YANG, Hanbiao; EVANCHIK, Marc; ZAHARIA, Cristiana A.; CAI, Haiying; HU, Lily W.; WO2014/8197; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 460-37-7, The chemical industry reduces the impact on the environment during synthesis 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, I believe this compound will play a more active role in future production and life.

To a solution of 2.0 g (6.60 mmol) of the compound from Ex. 38A in 35 ml of DMF were added 2.30 g (16.6 mmol) of potassium carbonate, and the mixture was stirred at RT for 15 min. Then 2.3 ml (20.0 mmol) of 1,1,1-trifluoro-3-iodopropane were added. Since the conversion was still incomplete after stirring at RT for 3 days, the mixture was first stirred at 50 C. for 4.5 h, and then a further 0.92 g (6.60 mmol) of potassium carbonate and 0.78 ml (6.0 mmol) of 1,1,1-trifluoro-3-iodopropane were added. The reaction mixture was then stirred at 60 C. overnight. After cooling to RT, the mixture was diluted with water and stirred for 30 min. The precipitated product was filtered off with suction, washed to neutrality with water and dried. 2.15 g (78% of theory) of the title compound were obtained, which was used for subsequent reactions without further purification. LC/MS (Method 2, ESIpos): Rt=1.08 min, m/z=397 [M+H]+.

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, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bayer Aktiengesellschaft; Bayer Pharma Aktiengesellschaft; HAERTER, Michael; KOSEMUND, Dirk; CANCHO GRANDE, Yolanda; DELBECK, Martina; KALTHOF, Bernd; LUSTIG, Klemens; SUESSMEIER, Frank; US2020/16159; (2020); 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. 847685-01-2, name is 4,5-Difluoro-2-iodoaniline, A new synthetic method of this compound is introduced below., Quality Control of 4,5-Difluoro-2-iodoaniline

4,5-Difluoro-2-iodoaniline (Intermediate 27, 1.24 g, 4.86 mmol) was dissolved in anhydrous DMF (15 mL). Pyruvic acid (1.32 g, 15 mmol) and DABCO (1.68 g, 15 mmol) were added and the mixture degassed by alternate vacuum and nitrogen purge. Palladium EPO acetate (56 mg) was then added and the mixture heated to 1000C. for 2h. After cooling to ambient temperature the reaction mixture was filtered through celite, diluted with ethyl acetate (10OmL), washed with 2M HCl (2x 2OmL) and water (2x 2OmL), dried (MgSO4) and evaporated to give the title compound as a dark solid (860 mg, 90%). 1H NMR delta: 7.0 (s, IH), 7.3 (dd, IH), 7.6 (dd, IH), 11.9 (s, IH); MS m/z 196 (m-H)

The synthetic route of 847685-01-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/82400; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 74-88-4, The chemical industry reduces the impact on the environment during synthesis 74-88-4, name is Iodomethane, I believe this compound will play a more active role in future production and life.

In 10 ml of N,N-dimethylformamide was dissolved 1.8 g (10.6 mmol) of 2-chloro-6-methylbenzoic acid, and then, 1.49 g (10.8 mmol) of potassium carbonate and 2.7 ml of methyl iodide were added to the solution, and the mixture was stirred at room temperature for 3 hours. After completion of the reaction, water was added to the reaction mixture and the mixture was extracted with diethyl ether. The organic layer was successively washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was applied to silica gel column chromatography (eluent: hexane/ethyl acetate=9/1(volume ratio)) to obtain 1.69 g of the title compound as pale yellowish liquid. CI-MS (m/z); 171 (M++1).1H-NMR (delta, CDCl3); 2.32 (s, 3H), 3.95 (s, 3H), 7.10 (t, J=4.3Hz, 1H), 7.22-7.23 (m, 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, Iodomethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Ube Industries, Ltd.; EP1408033; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 40400-15-5,Some common heterocyclic compound, 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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 suspension of (2-iodo-phenyl)-acetonitrile (Aldrich, 2.4 g, 10 mmol) and 2,3-difluorophenylboronic acid (Aldrich, 2.4 g, 15 mmol) in anhydrous methanol (10 mL) and toluene (20 mL) was added Cs2CO3 (9.8 g, 30 mmol). The mixture was degassed with nitrogen, followed by the addition of tetrakis(triphenylphosphine)palladium (1.2 g, 1 mmol). [0504] The reaction mixture was heated at 80 C. and stirred for 18 h. The mixture was cooled to room temperature and filtered through a short pad of silica gel. The silica gel was washed with ethyl acetate. The filtrate was concentrated. The residue was purified by chromatography (10-30% ethyl acetate in hexanes) to give the product ( 101) as a colorless oil (1.4 g, 62%)

The synthetic route of 40400-15-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wolkerstorfer, Andrea; Szolar, Oliver; Handler, Norbert; Buschmann, Helmut; Cusack, Stephen; Smith, Mark; So, Sung-Sau; Hawley, Ronald Charles; Sidduri, Achyutharao; Zhang, Zhuming; US2014/194431; (2014); 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. 2142-70-3, name is 1-(2-Iodophenyl)ethanone, A new synthetic method of this compound is introduced below., Recommanded Product: 1-(2-Iodophenyl)ethanone

The title compound (S6) was synthesized via modification to a general literature procedure.6 Aflame-dried Schlenk flask equipped with a magnetic stir bar was charged with anhydrouspotassium tert-butoxide (14.6 mmol, 1.64 g, 1.20 eq.) and methyltriphenylphosphonium bromide(14.6 mmol, 5.23 g, 1.20 eq.). The flask was placed under vacuum, backfilled with nitrogen, andthen placed in a 0C ice-water bath. Anhydrous THF (16 mL) was added down the side of theflask and the bright yellow mixture was stirred at 0C for 45 minutes. Then a solution of 2?-iodoacetophenone (12.2 mmol, 1.74 mL, 1.00 eq.) in anhydrous THF (8 mL) was added dropwise.The solution was gradually warmed to room temperature with stirring for 16 h. Thesolution was filtered, the filtrand washed with diethyl ether, and the resulting filtrateconcentrated in vacuo. The crude residue was purified by silica gel column chromatography(hexanes; Rf = 0.65) to provide the desired 1-iodo-2-(prop-1-en-2-yl)benzene (S6) as a clear,colorless oil in 89% yield (2.64 g).

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; Moyer, Brandon S.; Gagne, Michel R.; Synlett; vol. 28; 18; (2017); p. 2429 – 2434;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com