Month: May 2021

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. 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C7H5IO2

General procedure: 2-Phenylindole (408 mg, 2.0 mmol, 1 equiv), aryl iodide (2.0 mmol, 1 equiv), NaOt-Bu (288mg, 3.0 mmol,, 1.5 equiv), CNT-CuO (contained Cu 9.1 %, 70 mg, 5.0 mol%), were reacted in DMSO (10.0 mL) at 120 C for 12 h. The mixture charged to separating funnel added water, extracted with EtOAc. The organic layer washed with water many times for removing water, dried over magnesium sulfate. Evaporation of the solvent under reduced pressure provided the crude product, which was purified by column chromatography on silica gel.(eluent : hexane / ethyl acetate = 10 / 1).

The synthetic route of 5876-51-7 has been constantly updated, and we look forward to future research findings.

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. SDS of cas: 6940-76-7

(b) 4-(3-Chloro-propane-1-sulfonyl)-1,2-difluoro-benzene To 3,4-difluoro-benzenesulfinic acid (500 mg, 2.81 mmol) and triethylamine (0.43 ml, 3.10 mmol) in 10 ml DMF was added 1-chloro-3-iodopropane (1.43 g, 7.00 mmol) and the mixture heated at 65 C. for 3 h. The reaction mixture was then poured onto water and extracted three times with ethyl acetate. The combined organic phases were then washed with saturated aq. NaCl solution, dried over Na2SO4, and concentrated in vacuo. The residue was chromatographed over SiO2 (ethyl acetate/heptane 1:50) to afford the title compound (300 mg, 42%) as an off-white crystalline solid. MS (ISP): 257.2 {37Cl}MH+, 255.1{35Cl}MH+

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.

Adding a certain compound to certain chemical reactions, such as: 89488-57-3, name is 1,4-Diiodo-2-nitrobenzene, 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 89488-57-3, COA of Formula: C6H3I2NO2

(RS)-1-(4-Iodo-2-nitrophenyl)-2,2-dimethyl-1-propanol: Under a nitrogen atmosphere a solution of 1,4-diiodo-2-nitrobenzene (3.0 g, 8.0 mmol) in anhydrous THF (20 mL) was cooled to minus 40 C., and then a solution of phenylmagnesium chloride (2 M in THF, 4.8 mL, 9.6 mmol) was added dropwise at a rate that the temperature would not exceed minus 35 C. Upon completion of the addition the mixture was stirred for ten minutes, followed by addition of trimethylacetaldehyde (1.2 mL, 11.2 mmol), and the mixture was stirred for 30 minutes at minus 40 C. The mixture was gradually warmed up to room temperature, quenched with saturated ammonium chloride (60 mL), poured into water (120 mL), and extracted with ethyl acetate twice (60 mL each). The combined organic phase was washed with water (60 mL), dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography to yield racemic (RS)-1-(4-iodo-2-nitrophenyl)-2,2-dimethyl-1-propanol (2.17 g, 81%) as a brown oil. 1H NMR (400 MHz, CDCl3): delta 8.04 (d, 1 H, J=1.6 Hz, Ph-H), 7.88 (dd, 1 H, J=1.6 and 8.4 Hz, Ph-H), 7.51 (d, 1 H, J=8.4 Hz, Ph-H), 5.28 (d, 1 H, J=3.6 Hz, Ph-CH), 2.29 (d, 1 H, J=3.6 Hz, OH), 0.85 (s, 9 H, C(CH3)3). 13C NMR (100 MHz, CDCl3): delta 149.87 (C), 141.0 (CH), 136.2 (C), 132.3 (CH), 131.63 (CH), 91.85 (C), 74.33 (CH), 36.81 (C), 25.6 (CH3).

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Synthetic Route of 5876-51-7, 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 5876-51-7 as follows.

To toluene 3.0mL solution of tert-butyl 2-amino-4-phenethylbenzoate 0.10g were added 1-iodo-3,4-methylenedioxybenzene 0.14g, cesium carbonate 0.22g, tris(dibenzylideneacetone)dipalladium(0) 3mg and 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl 8mg, and it was stirred at 110C for 24 hours. After the reaction mixture was cooled to room temperature, tris(dibenzylideneacetone)dipalladium(0) 3mg and 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl 8mg were added to it, and it was stirred at 110C for 24 hours. After the reaction mixture was cooled to room temperature, ethyl acetate and 10% citric acid aqueous solution were added to it. The organic layer was separated and collected, dried over anhydrous magnesium sulfate after washing with saturated sodium chloride aqueous solution, and the solvent was removed under reduced pressure. The obtained residue was refined by silica gel column chromatography [Trikonex company, Flash Tube 2008, eluent; hexane:ethyl acetate=4:1] to give tert-butyl 2-((benzo-1,3-dioxol-5-yl)amino)-4-phenethylbenzoate. Trifluoroacetic acid 10mL was added to the obtained tert-butyl 2-((benzo-1,3-dioxol-5-yl)amino)-4-phenethylbenzoate, and it was stirred at room temperature for 2 hours. The solvent was removed under reduced pressure, and the obtained residue was refined by reversed-phase silica gel column chromatography [eluent; 80-100% acetonitrile/0.1% trifluoroacetic acid aqueous solution] to give 2-((benzo-1,3-dioxol-5-yl)amino)-4-phenethylbenzoic acid 12mg of white solid. 1H-NMR(DMSO-d6) delta value: 2.74-2.86(4H,m),6.03(2H,s),6.54(1H,dd,J=8.1,2.1Hz),6.61(1H,d d,J=8.1,1.5Hz),6.74(2H,d,J=2.1Hz),6.86(1H,d,J=8.1Hz),7. 13-7.20(3H,m),7.22-7.29(2H,m),7.77(1H;d,J=8.1Hz),9.40(1H,s),12.70-12.95(1H,broad).

According to the analysis of related databases, 5876-51-7, the application of this compound in the production field has become more and more popular.

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. 628-21-7, name is 1,4-Diiodobutane, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1,4-Diiodobutane

Stage 1 (0250) An oven-dried 3 L 4-neck flask fitted with an internal thermometer, N2 bubbler, overhead stirrer and oven-dried pressure-equalising dropping funnel was charged with 1,4-dibromo-2,5-dimethylbenzene (70 g, 265 mmol) and dry THF (700 mL). The solution was cooled with stirring to <-70 C. to produce a white slurry. s-Butyllithium (370 mL, 1.4 M, 518 mmol) was charged to the dropping funnel and added dropwise over the space of 2 h ensuring the reaction temperature did not exceed -70 C. The slurry was stirred for 2 h after which GCMS confirmed the lithiation was complete. The dropping funnel was charged with a solution of 1,4-diiodobutane (15.7 mL, 119 mmol) in dry THF (160 mL) which was then added dropwise over 0.75 h. The resulting pale yellow slurry was allowed to warm to room temperature and stirred for 12 h. The reaction was quenched by addition of water. The mixture was transferred to a separating funnel and the layers were separated. The aqueous layer was extracted with diethyl ether and the combined organics were washed with water, dried with MgSO4, filtered and concentrated to yield an off-white solid. The product was triturated with 300 mL methanol for 2 h and recrystallised from toluene/IPA to yield a white powder that was dried in the oven (31.86 g, 63%). GCMS indicated a purity of 96% and the material was taken to the next stage without further purification 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 628-21-7.

Some common heterocyclic compound, 450412-29-0, name is 1-Bromo-3-fluoro-2-iodobenzene, molecular formula is C6H3BrFI, 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

Pd(Pli3P)4 in a 500-mL round-bottom flask under N2 atmosphere is treated sequentially with a solution of l-bromo-3-fluoro-2-iodo-benzene (30 g, 0.1 mol) in toluene (250 mL), a solution of 2N aq Na2CO3 (200 mL) and 3-methyl phenylboronic acid in ethanol (62 mL). This mixture is heated at reflux under N2 for 12 h, then cooled to rt. The mixture is partitioned between water and EtOAc. The combined organic layers are washed with brine, dried over MgSO4, evaporated and purified by column chromatography to give 6-bromo-2-fluoro-3′-methyl-biphenyl (12 g). 1HNMR (400MHz, CD3OD): 7.03 (m, 2H), 7.48-7.04 (m, 4H), 7.50 (d, IH).b) 6-Bromo-2-chloro-3 ‘-methyl-biphenyl

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 450412-29-0, its application will become more common.

These common heterocyclic compound, 2401-21-0, name is 1,2-Dichloro-3-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. Recommanded Product: 2401-21-0

EXAMPLE 25A [(2,3-dichlorophenyl)ethynyl](trimethyl)silane 1,2-Dichloro-3-iodobenzene (4.95 g, 18.1 mmol), trimethylsilylacetylene (2 g, 20 mmol), bis(triphenylphosphine)palladium(II)chloride (245 mg, 0.35 mmol), and copper(I)iodide (45 mg, 0.24 mmol) were combined in triethylamine (120 mL) and heated at reflux for 45 minutes. The mixture was allowed to cool to room temperature and was then partitioned between diethyl ether and saturated sodium chloride. The organic phase was dried with sodium sulfate, filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was taken directly on to the next step.

The synthetic route of 1,2-Dichloro-3-iodobenzene has been constantly updated, and we look forward to future research findings.

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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8H6BrIO

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

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 31827-94-8.

Electric Literature of 202982-67-0, 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. 202982-67-0, name is 4-Chloro-3-fluoroiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a Schlenk tube, a solution of 4-Chloro-3-fluoroiodobenzene (7.3 g, 28.4 mmol), K3PO4 (16.1 g, 75.9 mmol), (S)-methylpyrrolidine-3-carboxylate (1271) hydrochloride (3.1 g, 19.0 mmol) and P(tBu)3 HBF4 (551 mg, 1.90 mmol) in dioxane (150 mL) was purged with N2 (3x). Pd(OAc)2 (213 mg; 0.95 mmol) was added and the reaction mixture was stirred at 100C for 16 h, then cooled down to rt. The mixture was diluted with EtOAc and water. The layers were separated. The aqueous layer was extrated with EtOAc (twice). The combined organic layers were washed with brine, dried over MgS04, filtered and the solvent was removed under reduced pressure. The residue was purified by preparative LC (irregular SiOH, 15-40 muiotaeta, 220 g Grace, liquid injection (Heptane), mobile phase gradient: from Heptane 100%, to heptane 70%>, EtOAc 30%>) to give 1.91 g (37%) of intermediate (U6) as an orange oil.

The synthetic route of 4-Chloro-3-fluoroiodobenzene has been constantly updated, and we look forward to future research findings.

391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, 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: 391211-97-5

To a stirred mixture of 3,4-difluoro-2-[(2-fluoro-4-iodophenyl)amino] benzoic acid (12 g, 30.5 mmol), prepared using procedures similar to those described in US 7,019,033, in dichloromethane (70 mL) at 0 C was added pyridine (2.5 mL, 30.8 mmol) followed by dropwise addition of cyanuric fluoride (2.8 mL, 33.6 mmol). The reaction mixture was stirred at 0 C for 10 minutes and then warmed to room temperature and stirred for 2 hours. The reaction mixture was diluted with water and extracted with dichloromethane (100 mL). The aqueous layer was extracted once with dichloromethane (50 mL). The combined organic layers were washed with saturated aqueous sodium bicarbonate solution, brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give crude product as a brownish solid. Crude product was purified by flash chromatography (plug, 25% ethyl acetate in hexanes) to afford 3,4-difluoro-2-[(2-fluoro-4-iodophenyl)amino] benzoyl fluoride as a beige solid (11.8 g, 97% yield). 1H NMR (400MHz, CD3OD): 8.41 (s, IH), 7.80-7.81 (m, IH), 7.52 (dd, IH), 7.43-7.47 (m, IH), 6.96-7.03 (m, IH), 6.85-6.92 (m, IH).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.