Month: May 2021

These common heterocyclic compound, 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile, 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. category: iodides-buliding-blocks

This reaction was performed under a nitrogen atmosphere. To a 100-mE reactor were added (-)-5-meth- ylmenthyl carboxylic acid (1R,25)-lla (450mg, 2.27 mmol) obtained in Synthesis Example 15, thionyl chloride (0.25 mE, 1.50 eq.), and a few drops of DMF, followed by stirring at room temperature for 3 hours. The solution in the system was distilled oil, and toluene (2 mE) was added thereto. The inside of the system was cooled to 100 C. or lower in an ice bath, and 4-aminobenzcyanide (900 mg, 3.0 eq.) was added slowly thereto. After two and a half hours, completion of the reaction was confirmed by GC-MS, and a post-treatment was performed. The reaction solution was transferred to a separating funnel and tap water and chloroform were added thereto to effect washing. The oil layer was washed twice with dilute hydrochloric acid, and thrther washed once with a saturated saline solution, and then dried with anhydrous magnesium sulfate. The resulting solution was concentrated under reduced pressure, and then isolation and purification were performed by column chromatography, whereby an amorphous solid was obtained (545 mg, yield: 77%, 80% cc.).10429] [a]D20=_20.6 (c=0.5, EtOH)HRMS: mass: 317.2202, actual measurement value: 317.2211 (Fl) ?H-NMR (500 MHz, CDC13): oe0.86 (d, 3H, J=7.0 Hz), 0.88-1.00 (m, 9H), 1.20-1.31 (m, 3H), 1.39-1.65 (m, 4H), 1.71-1.81 (m, 1H), 2.30 (td, 1H, J=11.8, 3.8 Hz), 3.70 (s, 2H), 7.26 (d, 2H, J=8.0 Hz), 7.32 (br, 1H), 7.56 (d, 1H, J=8.0 Hz)

The synthetic route of 2-(4-Iodophenyl)acetonitrile has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 620-05-3, name is (Iodomethyl)benzene, 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 620-05-3, category: iodides-buliding-blocks

General procedure: A solution of iodomethyl compound (30 mmol) and ionic liquid [bmpy]PF6 (15 mL) was taken in a round bottom flask, and then H5IO6 (36 mmol) and V2O5 (0.9 mmol) were added to reaction solution at r.t. Reaction content was heated at 70 C with continuous stirring for about 4-9 h. Reaction progress was monitored by means of TLC using EtOAc/n-hexane 1:9 as an eluent. After completion of reaction, the product was extracted with DCM (3 × 10 mL). The organic layer was isolated and washed with 5% NaHCO3 solution (3 × 10 mL) and water (3 × 10 mL) to make the pH neutral. Then, the organic layer was dried over Na2SO4 and filtered. The carbonyl compound was purified through recrystallization from hexane and ethyl acetate (solid product) or by distillation (liquid product). In some cases, column chromatography was required to purify product. In these cases, the solvent was removed followed by column chromatography using hexane/ethyl acetate (8:1) as eluent which afforded carbonyl compound (83-94%). The rest of the ionic liquid and the catalyst were recovered by decantation of aqueous hydrogen halide produced in the reaction and concentrated under vacuum. Fresh substrates were then recharged to the recovered catalytic system and then recycled under specified reaction parameters.

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 of 42861-71-2, A common heterocyclic compound, 42861-71-2, name is 3-Iodophenyl acetate, molecular formula is C8H7IO2, 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.

Step A Heck Coupling Trans-Ethyl-7-{[3-(3-Hydroxy-phenyl)-allyl]-methanesulfonyl-amino}-heptanoate To a solution of 7-(allyl-methanesulfonyl-amino)-heptanoic acid ethyl ester (250 mg, 0.86 mmol), 1-acetyloxy-3-iodo-benzene (225 mg, 0.86 mmol), and triethylamine (139 mL, 1 mmol) in DMF (3 mL) was added palladium acetate (25 mg). The reaction was heated to 80 C. under nitrogen for 24 h. The mixture was cooled to room temperature and aqueous sodium thiosulfate and CH2Cl2 were added. The aqueous solution was extracted with CH2Cl2 (2*) and the combined organic layers were washed with water (1*) and brine (1*). The organic solution was dried with MgSO4, filtered, and concentrated in vacuo. The product was purified by radial chromatography (hexanes to 25% EtOAc/hexanes) to afford the title compound of Step A (95 mg). 1H NMR (CDCl3 400 MHz) delta 6.88-7.34 (m, 4H), 6.53-6.60 (m, 1H), 6.13-6.20 (m, 1H), 4.10 (q, 2H), 3.95 (d, 2H), 3.17-3.21 (m, 2H), 2.85 (s, 3H), 2.24-2.31 (m, 2H), 2.31 (s, 3H), 1.56-1.62 (m, 4H), 1.27-1.33 (m, 4H), 1.23 (t, 3H).

The synthetic route of 42861-71-2 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. 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Iodo-1,3-dimethylbenzene

General procedure: Iodobenzene (1.2 mmol) and [Pd(pp3S4)(dba)] (1 mol %) were stirred in isopropanol (2.5 ml). Alcohol (1 mmol) followed by Cs2CO3 (5 mol %) were added to the above solution in the atmosphere of air. The mixture was heated to 80 C and the progress of the reaction was monitored by TLC. Rest of the procedure is same as described above.

According to the analysis of related databases, 608-28-6, the application of this compound in the production field has become more and more popular.

Electric Literature of 34270-90-1, 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 34270-90-1 as follows.

Preparation of Compounds 1002 – 1005: NaH (28.03 mg, 60%) was added into a solution of 2-(4-fluorophenyl)-5-hydroxy-N-methylbenzofuran-3-carboxamide (50 mg) and (E)-1,4-dibromobut-2-ene (75 mg) inPhH. The reaction was heated at 85C for 4 – 7 days. The reaction was quenched withMeOH and solvents were removed under vaccum to give a residue which was purified bypreparative HPLC._Compounds 1003 – 1015 and 2001 – 2005 were prepared using the sameprocedure for compound 1002, using the corresponding di-electrophiles. LC condition for compounds 1003 – 1015 and 2001 – 2005 was the same as for compound 1002.

According to the analysis of related databases, 34270-90-1, the application of this compound in the production field has become more and more popular.

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. 88-67-5, name is 2-Iodobenzoic acid, A new synthetic method of this compound is introduced below., Computed Properties of C7H5IO2

General procedure: Hydrazides (30-58) were synthesized by one pot conventionalmethod24 Benzoic acid or its derivative (10 mmol) was dissolvedin ethanol (20 mL). Sulfuric acid (3 N, 2 mL) was added and thereaction contents were refluxed for six hours. The reaction wasmonitored with TLC. After the completion of the reaction, the reactionmixture was neutralized by adding solid NaHCO3, and filteredto remove excess of NaHCO3. In the neutralized reaction mixture which contains ethyl ester, hydrazine monohydrate (1.5 mL,3 mmol) was added and refluxed for 3-6 h to complete the reaction.Ethanol and unreacted hydrazine were removed by distillationupto 1/3 volume. The reaction contents were cooled, filteredand recrystallized from methanol to obtain the desired hydrazidecrystals (see Supporting information).

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 of 13421-13-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 13421-13-1 name is 4-Chloro-2-iodobenzoic acid, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

2-Iodo-4-chlorobenzoic acid (10 g, 35.5 mmol) and HBTU (17.5 g, 46 mmol) were added to DMF (100 ml), followed by cyclopropylamine (2.6 g, 46 mmol) and DIPEA (17.5 ml, 92 mmol). The reaction was stirred overnight before being quenched with 2.0 NaOH (100 ml), extracted with DCM (3 x 200 ml), dried and solvent removed in vacuo to yield a dark yellow solid. This was passed through a pad of silica, eluting with DCM, the filtrate was concentrated in vacuo to yield a yellow solid. Ether (200 ml) Was added, the slurry was sonicated for 20 mins, iso-hexane (100 ml) was then added and the system was stirred for 10 mins, filtered and dried to give a colourless solid (9.3 g, 82%). NMR (CDCl3) 7.82 (s, IH), 7.34 (d, IH), 7.28 (d, IH), 5.99 (s, IH), 2.94 – 2.84 (m, IH), 0.91 – 0.84 (m, 2H), 0.71 – 0.66 (m, 2H); m/z 322.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-2-iodobenzoic acid, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 622-50-4, name is N-(4-Iodophenyl)acetamide, 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 622-50-4, Quality Control of N-(4-Iodophenyl)acetamide

General procedure: Under nitrogen atmosphere, Cu2O (10 mol %), DABCO (25 mol %), and a stirring bar were added into a 10 mL oven-dried sealed glass tube (as shown in Figure S1). Then NMP (0.5 mL), aryl iodides (0.125 mmol, 1.0 equiv.) and PhSiH3 (0.75 mmol, 6 equiv.) were injected by syringe. The tube was then sealed and CO2 (0.67 mmol, 5.4 equiv., 15 mL) as well as NH3 (0.67 mmol, 5.4 equiv., 15 mL) were injected by syringe after N2 was removed under vacuum. Finally, the mixture was stirred for 24 hr in a pre-heated-to-130 C alloyed block. After the reaction was finished, the tube was cooled to room temperature and the pressure was carefully released. The yield of were measured by GC analysis using dodecane as the internal standard or by flash chromatography on silica gel (petroleumether/ethyl acetate).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, N-(4-Iodophenyl)acetamide, and friends who are interested can also refer to it.

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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C7H4F3I

General procedure: General procedure: A 25 mL two-necked, round bottomed flask equipped with a water condenser, nitrogen gas inlet, Teflon coated magnetic stir bar, and a rubber septum port was charged with Pd(PPh3)4 (0.48 g, 3?5 molpercent), Cu(I)I (0.87 g, 4.6 mmol), and 10 mL of dry DMF. Next, 3-iodobenzotrifluorine (2.28 g, 8.30 mmol) was added to the solution via syringe. Then, 2 (3.93 g, 9.22 mmol) was slowly added to this solution by syringe. The reaction mixture was stirred 12 h at room temperature. To remove the ISnBu3-n, the reaction mixture was stirred with Cu(OAc)2 (3.36 g, 18.4 mmol) and 5 mL of extra DMF for 2 h. Alternately, dry KF (0.58 g, 9.9 mmol) was added to the reaction flask and the mixture was stirred overnight. The reaction mixture was then poured over water (25 mL) in a separatory funnel and extracted with ether (3× 25 mL). The combined ether layers were washed with water (2× 25 mL). The organic layer was dried over MgSO4, filtered, and the solvent was removed by rotary evaporation. The crude product was purified by silica gel column chromatography using hexanes as eluent to give 4 (2.90 g, 82percent isolated yield, Rf (hexanes) = 0.36, purity by GLPC analysis = 98percent): 19F NMR (CDCl3) ?63.4 ppm (s, 3F), ?143.3 ppm (dt, 1F, 3JFF = 122.6 Hz, 3JFH = 23.9 Hz), ?159.8 ppm (dt, 1F, 3JFF = 123.7 Hz, 4JFH = 4.6 Hz); 19F{H} NMR (CDCl3): ?63.4 ppm (s, 3F), ?143.3 ppm (d, 1F, 3JFF = 122.9 Hz), ?159.8 ppm (d, 1F, 3JFF = 123.4); 1H NMR (CDCl3): 7.9 ppm (s, 1H), 7.8 ppm (d, 1H, 3JHH = 7.9 Hz), 7.6 ppm (dd, 1H, 3JHH = 9.0 Hz, 3JHH = 7.8 Hz), 7.5 ppm (d, 1H, 3JHH = 7.7 Hz), 5.9 ppm (ddt, 1H, 3JHH = 17.0 Hz, 3JHH = 10.2 Hz, 3JHH = 6.4 Hz), 5.3 ppm (dm, 1H, 3JHH = 17.1 Hz), 5.2 ppm (dd, 1H, 3JHH = 10.1 Hz, 2JHH = 1.3 Hz), 3.3 ppm (ddddd, 2H, 3JHF = 23.3 Hz, 3JHH = 6.5 Hz, 4JHH = 5.3 Hz, 4JHH = 1.4 Hz, 4JHH = 1.3 Hz); 13C NMR (CDCl3): 151.51 ppm (dd, 1JCF = 251.6 Hz, 2JCF = 55.9 Hz), 146.00 ppm (dd, 1JCF = 225.2 Hz, 2JCF = 43.3 Hz), 131.11 ppm (qd, 2JCF = 32.0 Hz, 4JCF = 2.7 Hz), 130.96 ppm (dd, 3JCF = 1.9 Hz, 4JCF = 1.8 Hz), 130.64 ppm (dd, 2JCF = 25.8 Hz, 3JCF = 6.6 Hz), 129.03 ppm (d, 4JCF = 2.0 Hz), 128.35 ppm (ddm, 3JCF = 8.5 Hz, 4JCF = 1.4 Hz), 125.16 ppm (m), 124.04 ppm (q, 1JCF = 272.3 Hz), 122.11 ppm (m), 118.43 ppm (s), 32.13 ppm (d, 2JCF = 22.8 Hz); GC?MS, m/z (relative intensity): 248 (M+, 100.00), 213 (62.76), 201 (62.15), 179 (85.05), 177 (57.02) 164 (92.70), 159 (70.96), 151 (98.55); HRMS: C12H9F5 (calculated: 248.0624, observed: 248.0620).

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Electric Literature of 64248-58-4, These common heterocyclic compound, 64248-58-4, name is 1,2-Difluoro-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.

In a 50- mL RB-flask was added [3- (4-HYDROXYPHENYL)] propionic acid (1.66 g, [10.] 0 mmol), 3,4-difluoroiodobenzene (2.40 g, 10.0 mmol), copper (I) bromide (0.100 g), potassium carbonate (2.76 g, 20.0 [MMOL),] and [N-METHYL-2-PYRROLIDONE] (20 [ML)] as solvent. The mixture was stirred for 5 min at room temperature and then heated to [140 C] (oil bath). After being stirred for 12 hours at [140 C,] the reaction mixture was cooled to room temperature and diluted with [ETOAC] (100 mL). The diluted mixture was washed with citric acid (aq, 30 mL), water (3 x 50 mL, brine and dried over [MGS04. THE] removal of solvent in vacuo afforded crude which was purified by chromatography (0.901 g, [32%)] : [1H] NMR (400 MHz, CDCl3) 8 11.44-11. 06 (br, 1H), 7.24-7. 14 (m, 2H), 7.14-7. 00 (m, [1H),] 7.00-6. 86 (m, 2H), 6.86-6. 75 (m, 1H), 6.75-6. 61 (m, 1H), 2.94 (t, 2H, J = 7.6 Hz), 2.68 (t, 2H, [J = 7.] 6 Hz); ESMS [M/E] : 277.2 (M-H+).

Statistics shows that 1,2-Difluoro-4-iodobenzene is playing an increasingly important role. we look forward to future research findings about 64248-58-4.