Month: May 2021

156150-67-3, name is 2-Chloro-1-fluoro-4-iodobenzene, 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. Computed Properties of C6H3ClFI

General procedure: A solution of 4-cyano-1H-imidazole (1000 mg, 10.74 mmol), 4-iodo -2-(trifluoromethyl)pyridine (3800 mg,14 mmol), (1R,2R)-N1,N2-dimethyl cyclohexane -1,2-diamine (150 mg, 1.07 mmol), CuI (200 mg, 1.07 mmol) and Cs2CO3 (7000 mg, 21.5 mmol) in 20 mL anhydrous DMF was stirred at 100 oC for 2 hours. The reaction mixture was cooled to room temperature and poured into 200 mL water. The mixture was extracted with ethyl acetate (80 mL*3). The organic layer were combined, washed by brine, dried by Na2SO4 and evaporated. The crude product was purified by silica flash column to afford compound 2 as white solid(1.5 g, 59% yield).

The synthetic route of 156150-67-3 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. 619-58-9, name is 4-Iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Safety of 4-Iodobenzoic acid

To a solution of 4-iodobenzoic acid (2.0g, 1.0mmol), copper (I) iodide (1.7g, 1.13mmol), palladium chloride (0.02g, 0.15mmol) and triphenylphosphine (2.1g, 1.0mmol) in triethylamine (7ml), was added ethynyltrimethylsilane (1.2g, 1.5mmol) dropwise over 30min. The resulting reaction mixture was then refluxed at 80C for 24h under an atmosphere of argon and monitored by TLC. After the completion of reaction, as indicated by the complete disappearance of starting material on TLC, the mixture was cooled and filtered through a Buchner funnel. The volatile solvents were removed under reduced pressure. The resulting crude light brown coloured material was extracted into ether, washed with brine solution, dried over anhydrous sodium sulphate, and concentrated. Finally the silylated product was purified by column chromatography on silica gel with 3% ethyl acetate in hexane as an eluent yielding 86% of pure 4-[2-(trimethylsilyl)ethynyl]benzoic acid (2). Off white solid, 1.53g; IR: 2953, 2156, 1681, 1604, 1454, 1377, 1251, 858cm-1; 1H NMR (500MHz, CDCl3): 8.0 (d, J=8.6, 2H, Ar-H), 7.6 (d, J=8.4, 2H, Ar-H), 0.27 (s, 9H).

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 619-58-9.

Electric Literature of 4387-36-4, A common heterocyclic compound, 4387-36-4, name is 2-Iodobenzonitrile, molecular formula is C7H4IN, 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.

S1:100 mmol of the compound of the above formula (1), 200 mmol of the compound of the above formula (2), 0.4 mmol of palladium acetate, and 150 mmol of tetra-n-butylammonium bromide were added to an appropriate amount of the organic solvent N,N-dimethylacetamide (DMA) at room temperature. And 150 mmol of sodium carbonate, then stirred to raise the temperature to 120 ° C, and stirred at this temperature for 15 hours;After the reaction was completed, the reaction mixture was poured into a sufficient amount of ethyl acetate, and then washed with saturated brine, and the organic layer and aqueous layer were separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the organic layer obtained by ethyl acetate extraction were dried over anhydrous Na 2 SO 4 and evaporated under reduced pressure. The elution is carried out, the eluent is collected and the eluent is removed by evaporation.The compound of the above formula (3) is thus a white solid, the yield is 87.8percent;

The synthetic route of 4387-36-4 has been constantly updated, and we look forward to future research findings.

Related Products of 5876-51-7, The chemical industry reduces the impact on the environment during synthesis 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of tetrabutylammonium bromide (1.100 g, 3.33mmol), potassium acetate (0.586 g, 3.57 mmol), and palladium acetate (0.025 g, 0.11mmol) in DMF (20 mL) were added substituted iodobenzene (2.21mmol) and substituted styrene (2.44 mmol). The reaction mixture was recharged with argon and stirred at 80C for 5 h in a sealed tube. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl and concentrated in vacuo. The residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 10:3) to afford pure product.

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-Iodobenzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

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. 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane, A new synthetic method of this compound is introduced below., name: 1,1,1-Trifluoro-4-iodobutane

2-(2,4-Dichlorophenyl)-5-methyl-1-[4-(4,4,4-trifluorobutoxy)-phenyl]-1H-imidazole-4-carboxylic acid piperidin-1-ylamide l-Iodo-4, 4,4-trifluorobutane (376 mg, 1.58 mmol) was added dropwise to a suspension of 2-(2,4-dichlorophenyl)-1-(4-hydroxyphenyl)-5-methyl-1H-imidazole-4-carboxylic acid piperidin-1-ylamide, from Ex 2, Step 1 (351 mg, 0.79 mmol) and K2CO3 (218 mg, 1.58 mmol) in 50 ml acetone. The reaction mixture was refluxed overnight, cooled, filtered and concentrated. Flash chromatography (silica, hexane: EtOAc 1: 2) afforded 200 mg (46%) of the title compound as a white solid. ‘H NMR (CDC13) : 8 8. 0 (1H, broad s), 7.4-7. 2 (3H, m), 7.1-7. 0 (2H, m), 6.9-6. 8 (2H, m), 4.1-4. 0 (2H, m), 3.0-2. 9 (4H, m), 2.5-2. 2 (5H, m), 2.2-2. 0 (2H, m), 1.9-1. 7 (4H, m), 1.6-1. 4 (2H, m). MS m/z 578 (M+Na). HPLC: 99.4%.

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.

Adding a certain compound to certain chemical reactions, such as: 34883-46-0, name is 1-Iodo-2-phenoxybenzene, 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 34883-46-0, Quality Control of 1-Iodo-2-phenoxybenzene

In a 2L three-necked flask,Into 44.4g (150mmol, 1.0eq.) 2- iodo diphenyl ether,Dissolved with 1000 ml of chloroform,An additional 16.8 g (300 mmol, 2.0 eq.) of potassium hydroxide was added.95.85 g (600 mmol, 4.0 eq.) of liquid bromine was added dropwise at room temperature.After the completion of the dropwise addition, the reaction was stirred at room temperature for 12 hours.The reaction was quenched with a saturated Na 2 SO 3 solution, and a large amount of solid was precipitated, stirred, suction filtered, washed with water, washed with ethanol, and recrystallized from chloroform and ethanol.Finally, 50 g of Intermediate-1 was obtained in a yield of 73.3%.

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, 1-Iodo-2-phenoxybenzene, other downstream synthetic routes, hurry up and to see.

Electric Literature of 627-32-7,Some common heterocyclic compound, 627-32-7, name is 3-Iodo-1-propanol, molecular formula is C3H7IO, 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.

Example 33 2-Amino-6-({[2-(4-chlorophenyl)-1,3-thiazol-4-yl]methyl}sulfanyl)-4-[1-(3-hydroxypropyl)-1H-pyrazol-3-yl]pyridine-3,5-dicarbonitrile 50 mg (0.092 mmol) of the compound from Example 5 were dissolved in 0.8 ml of DMF, 15 mg (0.101 mmol) of DBU and 21 mg (0.111 mmol) of 3-iodopropanol were added and the mixture was stirred at 120 C. overnight. A little water and ethyl acetate were added to the mixture, and the two phases formed were separated. The aqueous phase was extracted twice with ethyl acetate. The combined organic phases were concentrated on a rotary evaporator and the residue was purified by thick-layer chromatography (toluene:acetonitrile=3:1). Yield: 18 mg (38% of theory) 1H-NMR (400 MHz, DMSO-d6): delta=8.10 (br s, 2H), 7.96-7.90 (m, 4H), 7.57 (d, 2H), 6.74 (d, 1H), 4.62 (s, 2H), 4.60 (t, 1H), 4.26 (t, 2H), 3.40 (q, 2H), 1.96 (Quintett, 2H). LC-MS (Method 2): Rt=2.54 min; MS (ESIpos): m/z=508 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Iodo-1-propanol, its application will become more common.

Electric Literature of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Synthesis of compound 6 (0048) 3-iodo-4-methyl-benzoic acid (compound 5:23.6 g, 0.09 mol) was added into THF (100 ml)and DMF (1 ml), then thionyl chloride (11.78 g, 0.099 mol) was added, rise the temperature to 60 C for 1 hour, evaporate the solvent, to give 3-iodobenzoyl chloride (compound 6), used directly for the next step.

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

Reference of 3032-81-3, These common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-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.

To a solution of 1 (10mg, 0.057mmol), 2 (31mg, 0.114mmol) and CS2CO3 (95mg, 0.29mmol) in DMF (lmL) were added 2 mg of Pd(dba)2 and 2 mg of Xantphos. The suspension was degassed under vacuum and purged with N2 several times. The mixture was stirred at 120 °C for lh. LCMS showed the SM was consumed completely. Then the reaction mixture was diluted with EA (5mL) and washed with brine (2mL) twice. The organic solution was dried over anhydrous Na2SO4, filtered, concentrated under reduced pressure and purified by p-TLC to give the desired compound Compound 120 (6mg, yield: 33.3percent). LCMS: m/z, 321.0 (M+H)+; 1HNMR:(d-CDCl3, 400MHz): delta 8.65(s, 1H), 7.67(t, J=7.2, 1H), 7.45(d, J=7.6, 1H), 7.27(t, J=6.0, 1H), 6.70(s, 1H), 6.23(d, J=1.2, 2H), 4.14~4.30(m, 4H).

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Application of 628-77-3, These common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, 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 [Reaction Scheme 1-5 obtained [Intermediate 1-e] 9.7 g in the reactor 300 mL (21 mmol), into a tetrahydrofuran 77 mL, was cooled to 0 . In potassium-tert-butoxide 7.1 g (63 mmol) slowly and stir. 10 minutes later, it was added dropwise a solution of 1,5-diiodopentane 10.3 g (32 mmol) in 10 mL tetrahydrofuran at 0 , and the temperature was raised to room temperature and stirred for 24 hours. Into water, then the organic layer was extracted and then concentrated under reduced pressure, the resulting solid was purified by recrystallization to obtain the compound [formula 2] 4.7 g (yield: 42.2%)

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