Month: May 2021

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. 58755-70-7, name is 1-Iodo-4-methoxy-2-nitrobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C7H6INO3

Compound 4 To a solution containing compound 3 (240 mg, 1.25 mmol) and 4-iodo-3-nitroanisole (345 mg, 1.24 mmol) were added PdCI2(PPh3)2 (44 mg, 5.0 mol %), and CuI (12 mg, 5.0 mol %) in TEA (15 mL). The mixture was stirred at 550C for 3 h, cooled, and filtered. The filtrate was concentrated under reduced pressure. Chromatography of the residue on silica gel (Hex:AcOEt = 100:40 (v/v)) gave 380 mg (88%) of compound 4.

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; THRESHOLD PHARMACEUTICALS, INC.; WO2006/57946; (2006); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 5460-32-2, These common heterocyclic compound, 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, 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.

A mixture of I (117.0 g, 590 mmol), 4-iodo-1,2-dimethoxybenzene (85.0 g, 590 mmol), Pd(OAc)2 (13.2 g, 59 mmol) and tri(o-tolyl)phosphine (36.0 g, 118 mmol) in triethylamine (3 L) was heated at 90° C. for 12 h. The mixture was cooled to room temperature and diluted with ethyl acetate (3 L). The organic phase was washed with brine, dried (MgSO4), and concentrated in vacuo to dryness. The crude product was purified by silica gel chromatography (0 to 40percent ethyl acetate/hexanes) to provide (la) as a brown oil (87.0 g, 73percent based on the recovered starting material). 1H NMR (300 MHz, CDCl3): delta 6.85 (s, 2H), 6.79 (s, 1H), 6.64 (s, 1H), 3.98-3.93 (m, 4H), 3.88 (s, 3H), 3.86 (s, 3H), 2.10-2.00 (m, 4H), 1.81 (s, 3H), 1.68 (d, J=12.9 Hz, 4H), 1.17 (s, 1H)

Statistics shows that 4-Iodo-1,2-dimethoxybenzene is playing an increasingly important role. we look forward to future research findings about 5460-32-2.

Reference:
Patent; Sequoia Sciences, Inc.; Williams, Russell B; Eldridge, Gary; Starks, Courtney M.; Guzzo, Peter Robert; Huang, Zhongping; (100 pag.)US9562031; (2017); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

116632-39-4, name is 5-Bromo-2-iodotoluene, 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. Recommanded Product: 116632-39-4

A mixture of 5-bromo-2-iodotoluene (25.0g, 0.1mol), NBS (36.6g, 0.1mol), and BPO (0.6g, 2.6mmol) were dissolved in 200mL of CCl4 and refluxed. The mixture was allowed to stir until the completion of the reaction, which was confirmed by thin layer chromatography (TLC) analysis (7h). When the reaction ended, a large amount of the floating succinimide produced in the reaction systems was filtrated off. The filtrate was evaporated to remove the solvent. The crude product was purified by column chromatography on silica with petroleum ether as the eluent to give 16.3g of a white solid 5-bromo-2-iodobenzyl bromide. Yield:50%; 1H NMR (600MHz, CDCl3): delta=4.52 (s, 2H, Ph-CH2), 7.21-7.59(m, 3H, Ar-H) ppm.

The synthetic route of 116632-39-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Guan; Jia; Zhang; Zhang; Ma; Lu; Lai; Lei; Dyes and Pigments; vol. 136; (2017); p. 873 – 880;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 619-58-9,Some common heterocyclic compound, 619-58-9, name is 4-Iodobenzoic acid, molecular formula is C7H5IO2, 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 resealable reaction tube, 4-iodobenzoic acid (10.0 g, 40.03 mmol) and furan-2- ylboronic acid (8.95 g, 80.06 mmol) were dissolved in degassed DMF (250 mL) and water (50 mL) at rt under nitrogen atmosphere. Pd(PPli3)4 (4.65 g, 3.99 mmol), K2CO3 (16.6 g, 120.09 mmol) were sequentially added to the above solution under nitrogen atmosphere. The resulting mixture was degassed by purging argon gas for 15 min, and reaction mixture was heated to 90C until completion of the reaction (TLC). The reaction mixture was cooled to rt, diluted with cold water and washed with ethyl acetate (3 x 30 mLl.The aqueous layer was separated and acidified to pH 3 with concentrated HC1, before extracting with EtOAc (100 mL x 2). The combined extract was washed with brine and concentrated under reduced pressure to get title compound (6.92 g, 92%) as light yellow solid. LCMS (m/: 187 (M-l)+.

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

Reference:
Patent; SALK INSTITUTE FOR BIOLOGICAL STUDIES; MITOKYNE, INC.; EVANS, Ronald; BAIGA, Thomas, J.; BOCK, Mark, G.; DOWNES, Michael; EMBLER, Emi, Kanakubo; FAN, Weiwei; KEANA, John, F.W.; KLUGE, Arthur, F.; NOEL, Joseph, P.; PATANE, Mike, A.; WO2014/165827; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 13421-13-1, 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. 13421-13-1 name is 4-Chloro-2-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) Synthesis of 4-chloro-2-(4-methoxyphenylthio)benzoic acid (Reference Example compound 2-1) [0185] 4-chloro-2-iodobenzoic acid (20.0 g), 4-methoxybenzenethiol (8.71 ml), potassium hydroxide (15.4 g), copper powder (0.48 g) and water (240 ml) was stirred under reflux for 4 hr. The reaction mixture was poured into a mixed solution of ethyl acetate and 1M hydrochloric acid, and the organic layer was separated. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was washed in diisopropyl ether and hexane (1:8) to give Reference Example compound 2-1 (18.8 g) as a white powder. 1H-NMR (CDCl3) delta (ppm) : 3.89 (3H, s), 6.69 (1H, d, J = 1.8 Hz), 7.01 (2H, d, J = 8.6 Hz), 7.09 (1H, dd, J = 2.0, 8.3 Hz, 7.50 (2H, d, J = 8.6 Hz), 8.04 (1H, d, J = 8.5 Hz).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-2-iodobenzoic acid, and friends who are interested can also refer to it.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; HAMADA, Maiko; TASHIRO, Kaoru; SAKASHITA, Hiroshi; KIUCHI, Masatoshi; TAKEDA, Shuzo; ADACHI, Kunitomo; EP2842937; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 25309-64-2, These common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-iodobenzene, 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: To astirred solution of: Aryl iodide (1.0 mmol), trans-4-Hydroxy-L-proline (1.5 mmol), nano CuFe2O4 (0.01 mmol), base (2 equiv), solvent (3.0 mL), 20h, 100 oC. The progress of the reaction was monitored by TLC. After the reaction was complete CuFe2O4 nano were placed on the bottom of the flask by a neodymium magnet, and the supernatant solution was removed. The crude residue was extracted with ethyl acetate (3 x 10 mL). The combined organic layers were extracted with water, saturated brine solution, and dried over anhydrous Na2SO4.The organic layers were evaporated under reduced pressure and the resulting crude product was purified by column chromatography to give the corresponding N-substituted pyrrole in excellent yields. The identity and purity of the product were confirmed by 1H,13C NMR, and mass spectra.

The synthetic route of 25309-64-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Satish; Reddy, K. Harsha Vardhan; Ramesh; Kumar, B.S.P. Anil; Nageswar; Tetrahedron Letters; vol. 55; 16; (2014); p. 2596 – 2599;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, molecular formula is C8H9IO2, 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. COA of Formula: C8H9IO2

General procedure: An argon-filled flask wasadd the respective aryl halide (1.0 mmol), CuI (20 mg, 0.1 mmol, 10 mol%), L3(37 mg, 0.1 mmol, 10 mol%), KOH (168 mg, 3 mmol), thiol (1.5 mmol) and glycerol(10 mL). The contents were then stirred at 100 C for 24 h. After that, themixture was cool to room temperature, diluted with ethyl acetate (20 mL) and washedwith saturated NaCl solution (3 x 20 mL). The organic layer was separated,dried over MgSO4 and concentrated under vacuum. The crude productwas purified by flash chromatography on silica gel using hexane /ethyl acetateas eluent

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 16932-44-8, its application will become more common.

Reference:
Article; Cargnelutti, Roberta; Lang, Ernesto S.; Schumacher, Ricardo F.; Tetrahedron Letters; vol. 56; 37; (2015); p. 5218 – 5222;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 13329-40-3,Some common heterocyclic compound, 13329-40-3, name is 1-(4-Iodophenyl)ethanone, molecular formula is C8H7IO, 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.

Dissolving 20 g (81 mmol) of 4′-iodo acetophenone into 200 milliliter of acetic acid, and adding 12.8 g (81 mmol) of bromine while cooling with ice, stirred at the temperature of 15 C for 3 hours. After the color of bromine disappeared, adding water and separating the precipitated solids by filtration, thereby obtained 27 g of crude 2-bromo-4′-iodo acetophenone.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(4-Iodophenyl)ethanone, its application will become more common.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1582516; (2005); A1;,
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. 16355-92-3, name is 1,10-Diiododecane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C10H20I2

1 molar parts taken honokiol and 2 moles of sodium carbonate were mixed in dry acetonitrile was added, the volume of acetonitrile and honokiol molar ratio of 150: 1 (L / mol), was added X (CH2)nY16 molar parts, at 85 for 5h was honokiol derivatives.However, the present embodiment of X (CH2)nThe Y, X, Y are I, n = 10.In other embodiments, X, Y independently is Br, O, S, F or Cl, n is an integer of ? 30 for 1,2,3,4, etc.

The synthetic route of 16355-92-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou card licensing Biological Technology Co., Ltd; Yuan, Xiao; Zhou, Dongbin; Fan, Jianjun; Zhang, Wei; (27 pag.)CN105622603; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 2468-56-6, 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 2468-56-6 as follows.

3) Synthesis of 6-trifluoroacetamido-1-hexyne To a solution of sodium hydride (60% oil, 2.55 g, 63.6 mol) in DMF (50 ml), trifluoroacetamide (8.99 g, 79.6 mmol) was added portionwise as about 10 portions with ice cooling. Subsequently, a solution of 6-iodo-1-hexyne (3.31 g, 15.9 mmol) in DMF (15 ml) was added to the reaction mixture. The reaction mixture was stirred at room temperature for four hours. The reaction mixture was added with saturated aqueous ammonium chloride (100 ml) and ether (100 ml) for extraction. The ether layer was dried over magnesium sulfate, and concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent; hexane-ethyl acetate mixed solvent) to afford 2.0 g of 6-trifluoroacetamido-1-hexyne (yield; 65.4%). Melting point: 41.0-42.5 C. 1H-NMR (270 MHz, CDCl3) delta ppm: 1.53-1.80 (m, 4H, -CH2(CH2)2-), 1.98 (t, 1H, J=2.7 Hz, H-CC-), 2.26 (dt, 2H, J=2.5, 6.7 Hz, CC-CH2-), 3.41 (q, 2H, J=6.8 Hz, CH2-N), 6.48 (brs, 1H, NHTfa)

According to the analysis of related databases, 2468-56-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; The Institute of Physical and Chemical Research; US6265569; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com