Tag: M.W=300-400

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. 628-77-3, name is 1,5-Diiodopentane, A new synthetic method of this compound is introduced below., Quality Control of 1,5-Diiodopentane

General procedure: To a diethyl ether (8.3mL) solution of ketone 6e (391mg, 1.61mmol) was dropwise added a toluene solution of potassium hexamethyldisilazide (0.50M, 3.40mL, 1.7mmol) at -78C. After stirring at 0C for 10min, the mixture was added to a diethyl ether (8.3mL) solution of 1,4-diiodobutane (0.43mL, 3.3mmol) and hexamethylphosphoramide (2.7mL) at -78C. The mixture was warmed to room temperature. After stirring for 7h, the reaction was quenched with phosphate buffer (pH 7). The organic materials were extracted with ethyl acetate three times. The combined organic extracts were washed with brine and dried over Na2SO4. After the solvent was removed under reduced pressure, the residue was purified by column chromatography (hexane/ethyl acetate=10/1) to give a crude mixture (372mg) including 8-iodo-1-phenyl-4-(3,3,3-trifluoroprop-1-en-2-yl)octan-3-one as a colorless oil. To a diethyl ether (3.1mL) solution of the obtained crude mixture was added dropwise a toluene solution of potassium hexamethyldisilazide (0.50M, 1.30mL, 0.65mmol) at -78C. After stirring at -78C for 5min, the mixture was warmed to room temperature and stirred for another 4h. The reaction was quenched with phosphate buffer (pH 7). The organic materials were extracted with ethyl acetate three times. The combined organic extracts were washed with brine and dried over Na2SO4. After the solvent was removed under reduced pressure, the residue was purified by column chromatography (hexane/ethyl acetate=10/1) to give 1h (257mg, 54%) as a colorless oil

The synthetic route of 628-77-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fujita, Takeshi; Hattori, Masahiro; Matsuda, Masaaki; Morioka, Ryutaro; Jankins, Tanner C.; Ikeda, Masahiro; Ichikawa, Junji; Tetrahedron; vol. 75; 1; (2019); p. 36 – 46;,
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. 121554-10-7, name is 5-Bromo-2-iodobenzonitrile, A new synthetic method of this compound is introduced below., Safety of 5-Bromo-2-iodobenzonitrile

T o a s o l u t i o n o f 5-bromo-2-iodobenzonitrile (5.0Og, 16 00mmoles) in anhydrous tetrahydrofuran (80ml) at -8O0C is added diisobutyl aluminium hydride (16.0ml, 16.0mmoles, 1 M solution in toluene) dropwise over 10 minutes. The reaction mixture is stirred at -8O0C for a 1 hour, then allowed to warm to ambient temperature and stir overnight. Additional diisobutyl aluminium hydride (16.0ml, 16.0mmoles, 1 M solution in toluene) is next added dropwise at room temperature, and the reaction mixture further stirred for 1hour. After careful quenching with 2M hydrochloric acid (cooling in ice bath), the crude product is extracted with ethyl acetate (x 2), then all organics are combined and dried over magnesium sulfate and filtered. The filtrate is evaporated under reduced pressure then purified by flash column chromatography (isohexane to 10% ethyl acetate in isohexane eluant) to afford 5-bromo-2- iodobenzaldehyde (0.85g).

The synthetic route of 121554-10-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA LIMITED; SCUTT, James Nicholas; WO2010/136431; (2010); 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. 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,4-Diiodo-2,5-dimethoxybenzene

Compound 4-1 (10.06 g, 25.8 mmol) was dissolved in 100 mL of dry dichloromethane,The reaction flask was then cooled in a dry ice acetone bath,A solution of 1 mol / L boron tribromide in dichloromethane (56.8 mL, 56.8 mmol) was slowly added dropwise,Natural warmingreaction4 days.100 mL of ice water was allowed to cool in an ice-water bath, and then the reaction solution was gradually dropped into it with stirring,Produce a lot of solid, standing. Filtered with a Buchner funnel, the solid was washed three times with ice water, dried in vacuo,To give white solid compound 5-1 (8.71 g, 24.1 mmol)Yield: 93%; characterization: white solid;

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; Shenzhen Da Wu Science And Technology Co., Ltd.; Wang Ziyu; Li Baojian; Qi Tafamingrenqingqiubugongkaixingming; (12 pag.)CN106496049; (2017); A;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 17024-12-3, name is 9-Iodophenanthrene, molecular formula is C14H9I, 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. HPLC of Formula: C14H9I

Mixed under argon flow were 100 g of N,N’-diacetyl-4,4′-benzidine (manufactured by Tokyo Kasei Kogyo Co., Ltd.), 337 g of 9-iodophenanthrene, 204 g of anhydrous potassium carbonate (manufactured by Tokyo Kasei Kogyo Co., Ltd.), 4.7 g of copper powder (manufactured by Hiroshima Wako Co., Ltd.) and 750 ml of decalin, and they were reacted at 190C for 3 days. After cooling, 2 liter of toluene was added thereto to filter an insoluble matter. The matter filtered was dissolved in 4.5 liter of chloroform to filter off an insoluble matter, and then the filtrate was treated with activated carbon and concentrated under reduced pressure. Acetone 3 litter was added when the solution became slurry in the middle of concentration, and crystal deposited was filtered and dried. This was suspended in a mixture of 2 liter of ethylene glycol and 20 ml of water, and 110 g of a 85 % potassium hydroxide aqueous solution was added thereto, followed by carrying out reaction at 120C for 12 hours. After left cooling down to a room temperature, the reaction liquid was injected to 4 liter of water and treated with activated carbon, and then it was concentrated under reduced pressure. Acetone was added when the solution became slurry, and crystal deposited was filtered and dried to obtain 116 g of N,N’-bis(phenantho-9-yl)-4,4′-benzidine (A3).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 17024-12-3, its application will become more common.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1559706; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 689291-89-2, name is 5-Bromo-2-iodobenzaldehyde, 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. Recommanded Product: 689291-89-2

To an oven-dried flask protected under a N2 atmosphere were charged compound 12 (540 mg, 1.74 mmol), trimethylsilylacetylene (0.68 g, 6.9 mmol), PdCl2(PPh3)2 (60 mg, 0.085 mmol), CuI (30 mg, 0.16 mmol), and Et3N (10 mL). The solution was bubbled by N2 at rt for 5 min and then heated to 60 C under stirring and N2 protection overnight. After the reaction was complete as checked by TLC analysis, the solvent was removed by rotary evaporation. The resulting residue was diluted with CHCl3. The mixture was filtered through a MgSO4 pad. The solution obtained was sequentially washed with HCl (aq. 10%) and brine. The organic layer was dried over MgSO4 and concentrated under vacuum to give crude 20, which was further purified by silica flash column chromatography (hexanes/CH2Cl2, 4:1) to yield compound 20 (518 mg, 1.74 mmol, 100%) as a colorless oil.

The synthetic route of 5-Bromo-2-iodobenzaldehyde has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhou, Ningzhang; Wang, Li; Thompson, David W.; Zhao, Yuming; Tetrahedron; vol. 67; 1; (2011); p. 125 – 143;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 811842-30-5, These common heterocyclic compound, 811842-30-5, name is 2-Bromo-1-fluoro-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.

Mix 2-bromo-1-fluoro-4-iodobenzene (18.0 g, 0.06 mol), Cu2O (36.0 mg, 0.25 mmol), and KOH (5.6 g, 0.10 mol) in 1,4-dioxane (20 ml) ), Under the protection of nitrogen, cyclopentathiol (5.1 g, 0.05 mol) was added to the system through a syringe, and the temperature was raised to 110 C. for overnight reaction. After the reaction solution was cooled to room temperature, ethyl acetate (30 ml) was added, and the filter cake was washed with ethyl acetate (20 ml). The filtrates were combined and concentrated to dryness under reduced pressure. The residue was separated by column chromatography to obtain the title compound (12.0 g, yield 72%).[1283]1H NMR (400MHz, CDCl 3) delta 7.62-7.49 (m, 1H), 7.34-7.20 (m, 1H), 7.09-6.95 (m, 1H), 3.52 (td, J = 7.2, 3.6Hz, 1H) , 2.08–1.92 (m, 2H), 1.85–1.56 (m, 6H).

The synthetic route of 811842-30-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JIANGSU HANSOH PHARMACEUTICAL GROUP CO., LTD.; SHANGHAI HANSOH BIOMEDICAL CO., LTD.; SU, Yidong; GU, Peng; CHEN, Xiaopo; LIU, Lei; BAO, Rudi; (192 pag.)WO2018/130174; (2018); 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. 54507-44-7, name is 2-Iodo-4-(trifluoromethyl)benzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 2-Iodo-4-(trifluoromethyl)benzoic acid

4) Synthesis of 2-[(3-chloro-4-methoxyphenyl)thio]-4-(trifluoromethyl)benzoic acid (compound 211-4) [0358] N,N-dimethylformamide (90 ml) was added copper powder (360 mg), and the mixture was stirred at 120C for 3 hr. The reaction mixture was cooled, 1M hydrochloric acid and ethyl acetate were added, an insoluble material was filtered off, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography and the obtained solid was washed with hexane to give compound 211-4 (12.6 g) as a white solid. 1H-NMR(DMSO-d6)delta(ppm):3.95(3H,s), 6.90(1H,s), 7.33(1H,d,J=8.6Hz), 7.55-7.61(2H,m), 7.71(1H,d,J=2.4Hz), 8.12(1H,d,J=8.6Hz), 13.8(1H,brs).

The synthetic route of 54507-44-7 has been constantly updated, and we look forward to future research findings.

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

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. 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,4-Diiodo-2,5-dimethoxybenzene

A two-neck round bottom flask (250ml) was cooled to -63 C in a liquid nitrogen/chloroform slush bath to which 1,4-diiodo 2,5-dimethoxybenzene (2.0g, 5.1mmol, 1.0 equiv) was dissolved in dichloromethane (40ml) under nitrogen. BBr3 (12ml, 1.0M, 12mmol) was then added dropwise through a septa seal using a syringe. The mixture was allowed to warm to room temperature and stirred for 24hrs and then carefully quenched with water (75ml). The aqueous layer was then extracted with ether (3 * 50ml). The combined organic phases were extracted with NaOH (150ml, 2N). The NaOH solution was then neutralized in dilute HCl in an ice bath to form a pink precipitate that was collected and dried. The resultant solid material was recrystallized from toluene to give light brown crystals, (1.48g, 80%).

The synthetic route of 51560-21-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tsakama, Madalitso; Shang, Yuting; He, Yonghuang; Fan, Bei; Wang, Fengzhong; Chen, Weihua; Dai, Xiaofeng; Tetrahedron Letters; vol. 57; 16; (2016); p. 1739 – 1742;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 503821-94-1, name is 3-Bromo-2-iodobenzoic 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 503821-94-1, Computed Properties of C7H4BrIO2

By the same procedure, using 3-bromo-2-iodo-benzoic acid as the starting material, 7-bromo-8-iodo-1,2,3,4-tetrahydroisoquinoline is prepared.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; SmithKline Corporation; US3988339; (1976); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 811842-30-5, These common heterocyclic compound, 811842-30-5, name is 2-Bromo-1-fluoro-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.

A solution of diisopropylethyamine (5 mL) and DMF (7 mL) was sparged with argon for about 15 minutes.1-(difluoromethoxy)-4-ethynyl-2-methylbenzene (1) (550 mg, 3.02 mmol) and 2-bromo-1-fluoro-4-iodobenzene (1.36 g, 4.53 mmol) were added to the reaction mixture and argon gas was bubbled for another 5 minutes. Copper(I)iodide (57.5 mg, 0.302 mmol) and PdCl2(PPh3)2 (106 mg, 151 mumol) were added to the reaction mixture and it was stirred at 60 C overnight. The mixture was diluted with ether and washed with water. The mixture was filtered over Celite and the organic layer was separated. The aqueous layer was back extracted with ether. The combined organic layers were washed with saturated ammonium chloride solution, dried using sodium sulfate, filtered and the solvent was evaporated under reduced pressure. The crude mixture was partitioned with hexane and water. Some undesired solids were removed by filtration. The organic layer was separated and dried using sodium sulfate. The filtrate was evaporated under reduced pressure. The crude mixture was purified by flash chromatography using hexanes as the eluent 2-bromo-4-((4-(difluoromethoxy)-3-methylphenyl)ethynyl)-1-fluorobenzene (2) (1.0 g, 93.3% yield).1H NMR (400MHz, DCM-d2) d = 7.79 (dd, J=2.0, 6.6 Hz, 1H), 7.50 (ddd, J=2.1, 4.7, 8.5 Hz, 1H), 7.46 (d, J=1.0 Hz, 1H), 7.40 (dd, J=2.0, 8.3 Hz, 1H), 7.17 (t, J=8.6 Hz, 1H), 7.10 (d, J=8.6 Hz, 1H), 6.82 – 6.41 (m, 1H), 2.33 (s, 3H).

The synthetic route of 811842-30-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORINIA; CAMPAGNA, Jesus; JOHN, Varghese; JAGODZINSKA, Barbara; (90 pag.)WO2019/169183; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com