Month: June 2021

Related Products of 3718-88-5, 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. 3718-88-5, name is 3-Iodobenzylamine hydrochloride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A suspension of 3-iodobenzylamine hydrochloride (4.95 g, 18.4 mrnol) in dichloromethane (100 mL) was treated with trieihylamine (3.1 mL, 22 mmol) and di-tert-butyl dicarbonate (4.40 g, 20 mmol) artid the resulting solution stirred at room temperature for 1.5 hours. The reaction fixture was then washed with 2M hydrochloric acid (30 mL), water (30 mL), cried over sodium sulfate and concentrated in vacuo to afford the title compound as a colourless solid in quantitative yield, 6.43 g. HNMR (400MHz, CDCI3) 8 : 1.46 (9H, s), 4.21-4. SO (2H, m), 4. 79-4. 89 (1 H, bs), 7.06 (1H, dd), 7.25 (1H, d), 7.60 (1H, d), 7.63 (1H, s); LRMS ESl m/z 332 [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, 3-Iodobenzylamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2005/92840; (2005); A1;,
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. 170112-66-0, name is 3,4,5-Trifluoroiodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 170112-66-0

Set up a reflux reaction device and put a stirrer into the reaction bottle. 4-propylbiphenylacetylene, 1,2,6-trifluoro-4-iodobenzene, Catalyst Pd(Pph3)4 and cuprous iodide; Replace the air in the sealing system with argon; inject triethylamine, Tetrahydrofuran, stir and slowly heat to reflux. Make sure the system reacts under argon protection. After 7 hours, the degree of reaction was measured by TLC. Step 2), purify the crude product of step 1) with a cable extractor: After the reaction is completed, the reaction solution is poured into ice water, and dilute hydrochloric acid is added dropwise and stirred. Drip into weakly alkaline; extract the above liquid with dichloromethane, collect the organic phase, The organic phase is washed twice with brine and then dried over anhydrous sodium sulfate or anhydrous magnesium sulfate Dry, finally, rotary evaporation of the dry organic phase to give a brown solid. At this time, the brown solid is the crude product of the sonoshihira reaction. Contains target products, self-coupling by-products, and other by-products. Set up the extraction device and pour it in the extraction bottle of the Soxhlet extractor. Into petroleum ether; the brown solid is placed in a filter paper tube, Place the filter paper tube in the extraction tube of the Soxhlet extractor; Heat and reflux for 1-2 hours, and cool the petroleum ether of the extraction bottle to room temperature or lower. The product solid precipitated and was filtered using a suction device. A product having a purity of 95% or more is obtained.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 170112-66-0.

Reference:
Patent; Shenzhen Chao Duowei Technology Co., Ltd.; Zhang Guoxian; Bao Rui; (18 pag.)CN106398714; (2018); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 260355-20-2, These common heterocyclic compound, 260355-20-2, name is 1-Chloro-4-iodo-2-(trifluoromethyl)benzene, 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.

The 1-chloro-4-iodo-2-trifluoromethylbenzene (10 mmol) obtained in the reaction 1.2 was dissolved in 20 ml of toluene, and the system was sequentially added with isoxazol-4-amine (12 mmol), palladium acetate ( 0.5 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (12 mmol), 3 ml of triethylamine. After stirring for 10 minutes, add 10 ml of cesium carbonate (10 mmol). The aqueous solution was heated to 50 C for 4 hours. After the reaction was completed, 20 ml of water was added to the system, stirred for 20 minutes, and the organic phase was dried over anhydrous sodium sulfate.Concentration and flash column chromatography gave 2.2 g of yellow N-(4-chloro-3-trifluoromethylphenyl)-isoxazole-4-amine powder, yield 84%.

The synthetic route of 260355-20-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhang Ruwei; Ge Baoyin; Jing Fan; Zhai Xuexu; (9 pag.)CN108633899; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 25245-27-6 as follows. Computed Properties of C8H9IO2

In a dry two necked flask were introduced N-{2-[1-(3,5-dimethoxyphenyl)-cyclohexa-2,5-dienyl]-ethyl}-4-methyl-benzenesulfonamide 3b (66 mg, 0.168 mmol), silvercarbonate (93 mg, 0.336 mmol), triphenylphosphine (6.6 mg, 0.025 mmol), 3,5-dimethoxyiodobenzene4b (89 mg, 0.336), palladium acetate (1.9 mg, 0.008 mmol) and acetonitrile (8.5mL). The mixture was warmed to 85C and stirred for 20 hours. The mixture was filteredthrough celite, which was then washed with ethyl acetate. Evaporation of the solvents led to apaste, which was purified through silica gel chromatography (Petroleum ether/EtOAc 80:20),affording 5b as a viscous oil (48 mg, 52%). IR (film, KBr, numax, cm-1): 2937, 1594, 1458, 1425,1325, 1204, 1155, 1064, 839, 732. 1H NMR (300 MHz, CDCl3): deltaH 1.38-1.50 (1H, m,CHaHxCH2N), 1.72-1.84 (2H, m, CHaHxCH2N and CH cyclopropane), 2.21-2.26 (1H, m, CHcyclopropane), 2.41 (3H, s, CH3 tosyl), 2.91 (2H, qa, 3JHH 7.3 Hz, CH2N), 3.28 (1H, broad s, CHcyclopropane), 3.77 (12H, 2OCH3 x 2), 4.46 (1H, broad s, NH), 5.20 (1H, d, 3JHH 5.3 Hz, CHolefinic), 5.82-5.84 (1H, m, CH olefinic), 6.22 (2H, s, 2CH aromatic) 6.32 (4H, s, 2CH x 2aromatic), 7.25 (2H, d, 3JHH 8.3 Hz, CH x 2 tosyl), 7.63 (2H, d, 3JHH 8.3 Hz, CH x 2 tosyl). 13CNMR (75.5 MHz, CDCl3): deltaC 21.6 (CH3 tosyl), 37.1, 38.0 (2CH cyclopropane), 38.1 (C,aliphatic), 41.2, 41.3 (2CH2, CH2CH2N), 51.2 (CH allylic), 55.4, 55.5 (2OCH3 x 2), 98.2, 98.5(2CH aromatic), 105.9, 110.0 (2CH x 2 aromatic), 127.1, 129.8 (2CH x 2 tosyl), 131.6, 134.2(2CH olefinic), 137.0, 140.0, 143.4, 146.7 (4C aromatic), 160.5, 161.0 (2C x 2 aromatic).MS(ESI) m/z (%): 1121 (2M+Na, 22), 588 (M+K, 13), 572 (M+Na, 100). HRMS calcd for[M+Na]+ C31H35NNaO6S: 572.2083; found 572.2082 (0 ppm).

According to the analysis of related databases, 25245-27-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Lebeuf, Raphael; Robert, Frederic; Landais, Yannick; ARKIVOC; vol. 2014; 3; (2013); p. 6 – 17;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 202982-67-0 as follows. name: 4-Chloro-3-fluoroiodobenzene

Tris(dibenzylideneacetone)dipalladium(0) (47.6 mg, 0.05 mmol), 2- (dicyclohexylphosphino)-2′,4′,6′-triisopropylbiphenyl (XPhos, 49.6 mg, 0.10 mmol), 4-chloro-3- fluoroiodobenzene (400 mg, 1.56 mmol, Aldrich), teri-butyl 2,6-diazaspiro[3.3]heptane-2- carboxylate, oxalic acid (300 mg, 1.04 mmol, ArkPharm), and cesium carbonate (1017 mg, 3.12 mmol) were suspended in dioxane (12 mL). The reaction mixture was stirred at 98 C for 18 hours and then cooled to ambient temperature. The crude reaction mixture was combined with 5 grams of Celite and concentrated under reduced pressure to a free flowing powder. The powder was directly purified by reversed-phase flash chromatography [Interchim PuriFlash C18XS 30 mupiiota 175 g column, flow rate 100 mL/minute, 5-100% gradient of acetonitrile in buffer (0.025 M aqueous ammonium bicarbonate, adjusted to pH 10 with ammonium hydroxide)] to give the title compound (0.27 g, 0.83 mmol, 79 % yield).JH NMR (400 MHz, DMSO-de) delta ppm 7.29 (t, J = 8.6 Hz, 1H), 6.42 (dd, J = 11.7, 2.6 Hz, 1H), 6.25 (ddd, J = 8.8, 2.6, 0.8 Hz, 1H), 4.01 (s, 4H), 3.94 (s, 4H), 1.38 (s, 9H); MS (ESI+) m/z 327 (M+H)+.

According to the analysis of related databases, 202982-67-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CALICO LIFE SCIENCES LLC; ABBVIE INC.; MARTIN, Kathleen Ann; SIDRAUSKI, Carmela; FROST, Jennifer M.; TONG, Yunsong; XU, Xiangdong; SHI, Lei; XIONG, Zhaoming; (165 pag.)WO2019/90090; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, molecular formula is C9H11I, 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. category: iodides-buliding-blocks

Specific operation: In a 25 mL reaction flask equipped with a magnetic stirrer, a metal catalyst palladium acetate (6.7 mg, 0.03 mmol), triphenylphosphine (20.0 mg, 0.075 mmol,) was added,S-2-bromophenyl-S-methyliminosulfanone (70.0 mg, 0.3 mmol), norbornene (56.4 mg, 0.6 mmol), potassium carbonate (82.8 mg, 0.6 mmol), nitrogen protection (at least three times nitrogen cycle)Acetonitrile (3 ml) and 2-iodoisopropylbenzene (88.6 mg, 0.36 mmol) were successively added under a stream of nitrogen.Closed container.The reaction was heated to 80 C for about 24 h, and the reaction was complete by TLC. After the first treatment, the reaction solution was diluted with 15 ml of ethyl acetate.Then, the catalyst and alkali and other inorganic substances are removed by suction filtration through a sand funnel containing silica gel.The resulting filtrate was separated by flash column chromatography to give the pure product 7-isopropyl-5-methyldibenzo[c,e][1,2]thiazine-5-oxide compound 3c.Yield: 40%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 19099-54-8, its application will become more common.

Reference:
Patent; Jiangxi Normal University; Chen Zhiyuan; Zhou Hao; Wang Xiumei; (17 pag.)CN107987034; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Recommanded Product: 628-77-3

Preparation of Intermediate methyl 1-(4-bromoDhenyl)cvclohexanecarboxylate (1AE-1); Sodium hydride (12 g, 52 mmol) was suspended in tetrahydrofuran (200 mL) under argon and warmed to 35C. Methyl 2-(4-bromophenyl)acetate (26mmol) in tetrahydrofuran added drop wise to reaction over 1 hour. The reaction mixture was then kept at this temperature for 1 hour until all gas evolution has ceased. The 1 ,5- diiodopentane (17 g, 52 mmol) was then added drop wise as a solution in tetrahydrofuran (100 mL) and the reaction mixture stirred at 35C for a further hour and at ambient temperature overnight. After this time, the reaction mixture was cooled to 00C and quenched by the addition of dry silica, filtered and the solvent removed under vacuum. The crude product was then purified by flash chromatography eluting with 33% ethyl acetate in heptane to give methyl 1-(4-bromophenyl)cyclohexanecarboxylate (1AC-1 ) (15.3 g, 99 % yield) as a yellow oil.1 H NMR (400 MHz, CDCI3): 7.45-7.38 (m, 2 H), 7.27-7.24 (m, 2 H), 3.63 (s, 3 H), 2.43 (d, J = 13.3 Hz, 2 H), 1.71-0.80 (m, 8 H) ppm.

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; PFIZER INC.; ASPNES, Gary, Erik; DOW, Robert, Lee; MUNCHHOF, Michael, John; WO2010/86820; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 20691-72-9, A common heterocyclic compound, 20691-72-9, name is 4-Iodo-2-nitroaniline, molecular formula is C6H5IN2O2, 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.

Method b To a mixture of the 4-iodo-2-nitroaniline (142 mmol) and cesium carbonate (55.5 g, 170 mmol) in 2-butanone (740 mL) was dropwise added a solution of Boc2O (37.8 g, 173 mmol) in 2-butanone (170 mL) and the resulting mixture was stirred at 52 C. for 26 h. The solvent was removed in vacuum, the residue was treated with a mixture of H2O (240 mL) and MeOH (240 mL) and extracted with hexane (3*500 mL). The combined hexane layer was washed with brine (200 mL) and all aqueous layers were reextracted with hexane (300 mL). All combined hexane layers were dried over MgSO4, filtered and the solvent was removed in vacuum to give an orange solid, which was purified by silica gel column chromatography with hexane/EtOAc to give the (4-iodo-2-nitro-phenyl)-carbamic acid tert.-butyl ester as a yellow solid.

The synthetic route of 20691-72-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; US6509328; (2003); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 13421-00-6, 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. 13421-00-6, name is 5-Chloro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

C. The starting 2-chloro-11H-dibenz(b,f)-1,4-oxathiepin is a novel compound which may be prepared by the following procedure: A solution of 120 g of 5-chloro-2- iodobenzoic acid (K. Pelz et al., Collect.Czech.Chem.Commun. 33, 1852, 1968) in 145 ml of tetrahydrofuran is stirred and treated at 10-20 C. for 45 minutes with 16.1 g of sodium borohydride. The mixture is then stirred for 30 minutes at this temperature and treated with a solution of 80.3 g (71.4 ml) of boron trifluoride etherate in 40 ml of tetrahydrofuran. It is stirred for another 3 hours and while cooling with ice-cold water it is decomposed at a maximum temperature of 8 C. with 50 ml of 5% hydrochloric acid added dropwise. It is diluted with water and extracted with benzene. The extract is washed with a 5% sodium hydroxide solution and water, dried with magnesium sulfate and evaporated. There are obtained 100 g (96%) of crude 5-chloro-2-iodobenzyl alcohol with m.p. of 115-117 C. The analytically pure substance is obtained by crystallization from ethanol; m.p. 116-117 C.

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-Chloro-2-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SPOFA, spojene podniky pro zdravotnickou vyrobu; US4431808; (1984); 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. 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,3-Difluoro-5-iodobenzene

Example 1.93: Preparation of 2-(((lr,4r)-4-((3-(3,5-Difluorophenyl)-3- phenylureido)methyl)cyclohexyl)methoxy)acetic Acid (Compound 44).; Step A: Preparation of 3,5-Difluoro-iV-phenylaniline.; In a 5 mL microwave reaction vial was placed aniline (0.298 g. 3.20 mmol) and 1,3- difluoro-5-iodobenzene (0.768 g, 3.20 mmol) in toluene (3 mL). KOH (0.323 g, 5.76 mmol) in water (650 muL) and N,N,N-trimethylhexadecan-l-ammium bromide (6.30 mg, 0.017 mmol) were added to the vial with stirring. After the reaction was warmed to 90 0C, bis[tri(f- butylphosphine]palladium[0] (0.016 g, 0.032 mmol) was added and the reaction was stirred at 150 0C for 4 h and then 160 0C for 2 h. The mixture was diluted with water and brine, and extracted with toluene. The toluene extract was subsequently washed with water, dried over MgSO4 and concentrated. The residue was purified by flash column chromatography to provide the title compound as a brown oil (0.132 g). LCMS m/z = 206.2 [M+H]+; 1H nuMR (400 MHz, DMSO-J6) delta ppm 6.54 (tt, J= 9.35, 2.27 Hz, IH), 6.63 (dd, J= 10.48, 2.15 Hz, 2H), 7.01 (dt, 7 = 14.65, 1.14 Hz, IH), 7.17 (dd, J= 8.59, 1.01 Hz, 2H), 7.34 (t, J= 7.83 Hz, 2H), 8.69 (s, IH).

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; ARENA PHARMACEUTICALS, INC.; WO2009/117095; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com