Month: April 2021

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. 620-05-3, name is (Iodomethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 620-05-3

General procedure: A mixture of benzyl bromide (171 mg, 1 mmol), diphenyl disulfide (131 mg, 0.6 mmol), PPh3 (184 mg, 0.7 mmol), and [pmIm]Br21 (94 mg, 0.4 mmol) was stirred at 75 C for 1.5 h (TLC). The reaction mixture was extracted with Et2O, and the organic layer was washed with brine (2 × 5 mL) and dried (Na2SO4). Evaporation of solvent left the crude product which was purified by column chromatography over silica gel (hexane) to afford the pure product, benzyl phenyl sulfide (168 mg, 84%) as a colorless liquid; IR (neat) 3058, 3028, 2923, 1581, 1495, 1479, 1452, 1438, 1238, 1090, 1068, 1024 cm-1; 1H NMR (300 MHz, CDCl3) delta 4.21 (s, 2H), 7.32-7.41 (m, 10H); 13C NMR (75 MHz, CDCl3) delta 39.5, 127.6, 128.0, 129.0 (2C), 129.3 (2C), 129.5 (2C), 130.3 (2C), 136.9, 137.9. The spectroscopic (FT-IR, 1H NMR and 13C NMR) data are in good agreement with the reported values.9b The remaining ionic liquid was washed with ether, dried under vacuum, and reused five times without appreciable loss of catalytic activity.

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 620-05-3.

Electric Literature of 5876-51-7,Some common heterocyclic compound, 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, 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.

[00200] To 21.9 mg NiCl2(dppf) in a reaction tube under nitrogen were added 4 ml dioxane, 0.42 ml (3 mmol) triethylamine, 0.22 ml (1.5 mmol) pinacolborane and 238 mg (0.96 mmol) 1-iodo-3,4-methylenedioxybenzene. The green coloured reaction solution was warmed to 80 C. with stirring for 6 h in an oil bath. An aliquot (ca. 0.3 ml) of the reaction solution was removed, extracted into diethyl ether and washed several times with water and analysed by gc (fid detector, SGE HTS capillary column). Besides a little 1,3-benzodioxole, the only other product peak in the gc was that due to the desired arylboronic acid pinacol ester. NiCl2 (dppf) was also shown to catalyse the formation of the desired product in acetonitrile.

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 766-99-4 as follows. HPLC of Formula: C8H5I

To a solution of l-ethynyl-4-iodobenzene 6 (0.908 g, 3.98 mmol) in THF (20 mL) at -78 0C was added ethylmagnesium bromide (3M in ether, 1.39 mL, 4.18 mmol). After 10 minutes the cooling bath was removed and the solution was allowed to stir at room temperature for 1 hour. The reaction mixture was then re- cooled to 0 0C and added to a solution of N-(tert-butoxycarbonyl)-L-proline N’- methoxy-N’-methylamide 2 (0.970 g, 3.76 mmol) in THF (10 mL). The reaction mixture was warmed to room temperature and stirring was continued for 12 hours before the mixture was quenched with saturated NH4Cl. The mixture was diluted with ethyl acetate/H2O, the layers separated and the aqueous phase was re-extracted with ethyl acetate (2x). The combined organic layers were washed (H2O, brine), dried (Na2SO4), and filtered, and the solvent was removed in vacuo. The resulting residue was purified by flash chromatography (hexane: ethyl acetate, 4: 1) to give (S)- tert-butyl 2-(3-(4-iodophenyl)propioloyl)pyrrolidine-l-carboxylate 7 (0.908 g, 71%) as a yellow oil which solidified on standing. 1H NMR (400 MHz, CDCl3) delta 7.72 – 7.76 (m, 2H), 7.26 -7.30 (m, 2H), 4.49 (dd, J=S. S, 4.3 Hz, 0.3H), 4.29 (dd, J=8.5, 5.5 Hz, 0.7 H), 3.59 (app t, J=6.7 Hz, 2H), 2.20 – 2.33 (m, IH), 1.85 – 2.10 (m, 3H), 1.45, 1.40 (s, 9H, rotamers in 2:3 ratio). LCMS: Anal. Calcd. for Ci8H20INO3: 425; found: 326 (M+H-Boc)+.

According to the analysis of related databases, 766-99-4, 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. 146137-72-6, name is 2-Fluoro-6-iodobenzaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H4FIO

Step 2: To a solution of 2-fluoro-6-iodobenzaldehyde (1.5 g, 6.0 mmol) and 2-bromopyridine-3, 4- diamine (1.1 g, 6.0 mmol) in ethanol (20 mL), was added ferric chloride (778 mg, 4.80 mmol). The reaction mixture was stirred at 60 C under oxygen atmosphere overnight. The next day, solvent was evaporated via rotavap and theresulting residue was purified by column chromatography on silica gel eluting with petroleum/ethyl acetate (3 :1) to give the desired product (1.6 g, 64% yield) as a yellow solid. LCMS (ESI) m/z: 418 [M+H+].

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 146137-72-6.

Electric Literature of 620621-48-9, A common heterocyclic compound, 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, molecular formula is C8H6ClIO2, 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.

8.1 2-Chloro-5-(pyrimidin-4-ylamino)-benzoic acid methyl ester Sodium phenoxide (810 mg), tris(dibenzylideneacetone)dipalladium (0) (102 mg), Xantphos (161 mg) and methyl-2-chloro-5-iodobenzoate (1379 mg) were placed in a flask and flushed with argon. 4-aminopyrimidine (486 mg) and dioxane (27.5 mL) were added and the reaction mixture was heated to 120 C. for 18 h. After cooling to RT, it was diluted with EtOAc and washed with a 1M solution of NaOH. The organic phase was dried over MgSO4 and concentrated in vacuo. The crude material was purified by CC (Hept/EtOAc 1/1 to 0/1) to give 718 mg of the titled compound as a yellowish powder. LC-MS (B): tR=0.48 min; [M+H]+: 264.21.

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.

Electric Literature of 689260-53-5, A common heterocyclic compound, 689260-53-5, name is 2-Bromo-5-iodo-1,3-dimethylbenzene, molecular formula is C8H8BrI, 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 2-bromo-5-iodo-1,3-dimethylbenzene (300 mg, 0.965 mmol), 1-aminocyclopropane carboxylic acid (195 mg, 1.93 mmol), copper iodide (I) (37 mg, 0.194 mmol), and diazabicycloundecene (0.50 mL, 3.35 mmol) in dimethylacetamide (2.6 mL) was stirred at 120C for three hours under nitrogen atmosphere. The reaction mixture was purified by silica gel column chromatography (Wakosil C18, acetonitrile – water (0.1% formic acid)) to afford 1-((4-bromo-3,5-dimethylphenyl)amino)cyclopropane carboxylic acid (219 mg, 80%). MS(ESI) m/z = 284, 286 (M+H)+.

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.

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 916792-62-6 as follows. Formula: C7H3FIN

Intermediate 50: 3-Fluoro-2-(pyrimidin-2-yl)benzoic acid.Step A: 3-Fluoro-2-(pyrimidin-2-yl)benzonitrile. 2-lodo-3- fluorobenzonitrile (2.5 g, 10.3 mmol) and 2-tributylstannane pyrimidine (3.7g, 10.0 mmol) were combined and dissolved in degassed DME (18 ml) then purged with bubbling N2 for 5 minutes. The reaction was treated withPd(PPh3)4 (577 mg, 0.5 mmol) and then purged with bubbling for 5 minutes in a sealed vessel and then heated in microwave at 160 C for 90 min. The reaction was cooled and filtered through celite and concentrated to minimum volume and the ppt the formed was diluted with hexanes (40 ml) and cooled to 0 C then filtered. The solid purified (FCC) (20-100% EA / hex) to give 3-fluoro- 2-(pyrimidin-2-yl)benzonitrile. 1 H NMR (400 MHz, CDCI3): 8.93 (d, J = 4.9 Hz, 2H), 8.14 (dd, J = 9.6, 2.7 Hz, 1 H), 7.86 (dd, J = 8.6, 5.3 Hz, 1 H), 7.36 (t, J = 4.9 Hz, 1 H), 7.32 – 7.24 (m, 1 H).

According to the analysis of related databases, 916792-62-6, 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: 33994-44-4, name is Methyl 3-(4-Iodophenyl)propanoate, 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 33994-44-4, name: Methyl 3-(4-Iodophenyl)propanoate

A 500 ml three-neck flask is charged with 14.0 g of 4-(2-thienyl)acetoanilide, 22.4 g of methyl 4-iodophenylpropionate, 13.4 g of potassium carbonate, 0.8 g of copper sulfate pentahydrate and 40 ml of o-dichlorobenzene, and the mixture is stirred under heating at 200 C. for 15 hours in a nitrogen stream. After this reaction, 100 ml of ethylene glycol and 5.4 g of potassium hydroxide are added to the reaction mixture, which is then refluxed under heating for 3 hours in a nitrogen stream, then cooled to ambient temperature, poured into 300 ml of distilled water and neutralized by hydrochloric acid to thereby precipitate crystals. The crystals are filtered, sufficiently washed with water and then transferred to a 1 L flask. To the crystals is added 500 ml of toluene, followed by refluxing under heating to remove water by azeotropic distillation. Then, 100 ml of methanol and 1 ml of concentrated sulfuric acid are added thereto, and the resulting mixture is refluxed under heating for 2 hours in a nitrogen stream. After the reaction, the reaction solution is dissolved in distilled water and extracted with toluene. The organic phase is sufficiently washed with distilled water. Next, the organic phase is dried by sodium sulfate anhydride, a solvent is evaporated off under reduced pressure and the residue is recrystallized from an ethyl acetate-hexane mixed solution to thereby obtain 15.1 g of diarylamine. A 100 ml flask is charged with 5.5 g of the thus-obtained diarylamine, 3.2 g of 4,4-diiodobiphenyl, 2.2 g of potassium carbonate, 0.2 g of copper sulfate pentahydrate and 10 ml of o-dichlorobenzene, and the mixture is refluxed under heating for 9.5 hours in a nitrogen stream. After the reaction is completed, the reaction mixture is cooled to ambient temperature and dissolved in 100 ml of toluene, and unnecessary substances are removed by filtration. An obtained filtrate is purified by silica gel column chromatography using toluene, to thereby yield 6.2 g of a thiophene-containing compound (Exemplary Compound 7). A melting point of the resulting thiophene-containing compound is 110 to 112 C. The IR spectrum (obtained using a KBr tablet method) of the thiophene-containing compound is shown in FIG. 2. An 1H-NMR spectrum (in a CDCl3 solvent) of the thiophene-containing compound is shown in FIG. 3.

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, Methyl 3-(4-Iodophenyl)propanoate, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, 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 199786-58-8, Product Details of 199786-58-8

To a stirred mixture of alcohol 2-iodo-5-bromobenzyl alcohol (9.14 g, 29.2 mmol) in of CH3Cl (150 mL) under argon was added 1M PBr3 in CH2Cl2 (35.0 mL, 35.0 mmol). The reaction mixture was stirred at room temperature for 20 minutes and then poured into a mixture of ice and saturated NaHCO3 solution (300 mL). The pH was adjusted to basic by addition of solid NaHCO3. This aqueous layer was extracted with EtOAc (1×600 mL, 2×400 mL). The combined EtOAc extracts were washed with brine (1×100 mL). The organic layer was dried (MgSO4), filtered and concentrated in vacuo to give 2-iodo-5-bromobenzyl bromide (5.69 g, 52%). 1H NMR (CDCl3): delta=7.68 (d, 1H, J=8.80 Hz), 7.59 (s, 1H), 7.18 (d, 1H, J=8.80 Hz), 4.51 (s, 2H). HPLC: Rt=3.87 min.

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-Bromo-2-iodophenyl)methanol, other downstream synthetic routes, hurry up and to see.

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 573764-31-5 as follows. name: 4-Chloro-3-iodoaniline

General procedure: A mixture of compound 3 (5 mmol), phenylboronic acid (10 mmol), Pd(Ph3P)4 (0.1 mmol), Na2CO3 (10 mmol) in 1,4-dioxane/H2O (20 mL) was stirred at 110 °C for 24 h under Ar. The reaction mixture was filtered through celite. The filtrate was concentrated in vacuo and then extracted with EtOAc. The organic layer was evaporated to give a residue, which was purified by chromatography (petroleum ether/EtOAc, 10:1) to give pure product as a yellow liquid, yield 88percent.

According to the analysis of related databases, 573764-31-5, the application of this compound in the production field has become more and more popular.