Tag: M.W=200-300

Application of 52570-33-9, 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. 52570-33-9 name is Methyl 3-iodo-2-methylbenzoate, 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.

Process using Pd Catalyst Under a nitrogen atmosphere, palladium acetate (223 mg, 0.99 mmol) , 4, 5-bis (diphenylphosphino) -9, 9-dimethylxanthene (Xantphos) (575 mg, 0.99 mmol) and toluene (62 ml) were mixed, and the mixture was stirred at room temperature for 15 minutes. To this solution, 2-amino-3-bromo-5-methylpyridine (6.20 g, 33.15 mmol), methyl 3-iodo-2-methylbenzoate (9.15 g, 33.15 mmol) and cesium carbonate (15.12 g, 46.41 mmol) were added. The mixture was stirred at an internal temperature of 100 to 105C for 7 hours. The reaction solution was cooled to room temperature, and water (50 ml) and toluene (50 ml) were added thereto. The organic layer was separated and washed sequentially with water (40 ml) and 10% brine (40 ml) . Silica gel (6 g) was added to the organic layer, the mixture was filtered, and the filtrate was concentrated under reduced pressure. Ethyl acetate (0.5 ml) and n-hexane (6 ml) were added to the concentrate, and the mixture was stirred at room temperature for 30 minutes. The crystals were collected by filtration, washed with ethyl acetate/n-hexane (1/12, 5 ml), and dried under reduced pressure at 40C, to yield the title compound (4.81 g) (yield 43.3%). 1H-NMR (CDCl3, TMS, 300 MHz) delta (ppm) : 2.23 (3H, s) , 2.52 (3H, s), 3.91 (3H, s), 6.78 (IH, brs) , 7.27 (IH, t, J = 8.0 Hz), 7.57-7.62 (2H, m) , 7.95 (IH, d, J = 1.1 Hz), 8.10 (IH, dd, J = 1.0 Hz, 8.1 Hz) .High resolution mass spectrometry Theoretical value: 334.0317 [M+] Measured value: 334.0313 [M+]Melting point: 63.9 to 64.7C

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-iodo-2-methylbenzoate, and friends who are interested can also refer to it.

Reference of 3930-83-4, These common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, 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.

General procedure: To a 25ml Schlenk tube containing a solution of 1 in 2ml of THF was added amide (1.0 mmol) and (EtO)3SiH (0.50 g, 3.0 mmol). The reaction mixture was stirred at 60 C until there was no amide left (monitored by TLC and GC-MS). The product was purified according to literature procedures by Beller [27].

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Related Products of 103962-05-6, 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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Under an argon atmosphere, nickel oxide (0.1 mmol, 10 molpercent), triphenylphosphine (0.2 mmol, 20 molpercent), iminodibenzyl substrate (1 mmol), potassium tert-butoxide (2 mmol, 2.0 equiv) were sequentially 4-trifluoromethoxyhalogenated aromatic hydrocarbon (2 mmol, 2.0 equiv) and tetrahydrofuran (2 mL) were added to a 10 mL sealed tube and placed in a 100° C. oil bath with heating and stirring for 24 hours. The reaction was completed and the reaction was exposed to air quenching. , and then directly separated by column chromatography to obtain amine products.According to the results of column chromatographic separation, the yields of 4-trifluoromethoxybromobenzene and 4-trifluoromethoxy iodobenzene respectively reacted with the substrate were 78percent and 69percent, respectively;

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-4-(trifluoromethoxy)benzene. I believe this compound will play a more active role in future production and life.

39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, 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. COA of Formula: C7H6FI

To a solution of 2-fluoro-4-iodotoluene (2.83 g, 12 mmol) in Cd4 (120 mL) were added NBS (2.24 g, 12.6 mmol) and BPO (0.06 g, 0.24 mmol). The reaction mixture was refluxed for 9 h under N2, then cooled to rt and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE) to give the title compound as a white solid (2.16 g, 57%).

The synthetic route of 39998-81-7 has been constantly updated, and we look forward to future research findings.

Reference of 39998-81-7, 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 39998-81-7 as follows.

2-Fluoro-4-iodobenzoic acid (Compound B) A round bottom (RB) flask containing a solution of 8.0 g (27.0 mmol) of sodium dichromate in 44 mL of glacial acetic acid was placed in an external water bath (21 C.) and left exposed to air. To the resultant orange slurry was added 3.2 g (13.6 mmol) of 2-fluoro-4-iodotoluene followed by the dropwise addition of 22 mL of c. sulfuric acid via syringe (caution: if added too quickly there is a tendency for the mixture to erupt). After the addition of approximately 8 mL of sulfuric acid, a green solid precipitated and the water bath temperature had risen (25 C.). The green reaction mixture was heated in an oil bath (90 C.) for one hour, allowed to cool to ambient temperature, diluted with 1N NaOH solution (aq.) and ethyl acetate (500 mL) and then quenched with sat. NaHCO3 (aq.) solution. The organic phase was separated and washed with water and brine, dried over MgSO4, filtered and concentrated in vacuo to an orange oil. Residual acetic acid was removed by further extraction between ethyl acetate and sat. NaHCO3 (aq.) solution and washing of the organic phase with water and brine. The organic phase was dried over MgSO4, filtered and concentrated in vacuo to give the title compound as an orange solid. PMR (DMSO-d6): delta 7.61 (1H, t, J=8.0 Hz, J (C–F)=8.0 Hz), 7.67 (1H, dd, J=1.5, 8.2 Hz), 7.78 (1H, dd, J=1.5 Hz, J (C–F)=8.9 Hz).

According to the analysis of related databases, 39998-81-7, the application of this compound in the production field has become more and more popular.

These common heterocyclic compound, 887266-99-1, name is 3-Fluoro-4-iodobenzonitrile, 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. HPLC of Formula: C7H3FIN

A mixture of 3-fluoro-4-iodobenzonitrile (1.0 g, 4.06 mmol), trimethylsilyl acetylene (0.595 g,6.07 mmol), CuT (50 mg, 0.26 mmol), PdC12(PPh3)2 (50 mg, 0.07 1 mmol) and TEA (3 mL) in DMSO (7 mL) was stirred at RT for 16 h. After the reaction, the reaction mixture was quenched with water, extracted with EtOAc. The organic layer was washed with water, brine, dried over Na2SO4 and concentrated to afford 750 mg of crude 2-chloro-5-((trimethylsilyl)-ethynyl) benzoate. To this crude solution of 2-chloro-5-((trimethylsilyl)ethynyl)benzoate (500 mg, 1.87 mmol) in DCM (10 mL) was added TBAF (1.0 g, 3.83 mmol) and stirred further at RT for h. Then the reaction mixture was quenched with water, extracted with DCM, washed with water, brine, dried over Na2SO4 and concentrated to afford 450 mg of the title product. ?H NMR (300 MHz, CDC13): 7.61-7.56 (t, J= 7.2 Hz, 1H), 7.44-7.38 (d, J= 8.1 Hz,2H), 3.52(s, 1H).

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

Electric Literature of 1450754-38-7, 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. 1450754-38-7 name is 3-(But-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine, 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.

K2CO3 (0.207g, 1.5 mmoL) and L3 (0.248g, 1.0 mmoL) were added orderly to a solution of phenol (0.113g, 1.2 mmoL) in DMF (10mL). The reaction mixture was stirred at 50C for 16h and monitored by TLC. The reaction was quenched by adding H2O (5mL). The crude product was exacted into EtOAc (3×10mL). The combined organic layers were washed with brine (10mL), and dried over Na2SO4 and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by flash column chromatography giving NP as colorless oil (171mg, yield 80%). 1H NMR (300MHz, CDCl3) delta 7.34-7.28 (m, 2H), 7.01-6.95 (m, 1H), 6.94-6.88 (m, 2H), 3.85 (t, J=6.2Hz, 2H), 2.13-2.06 (m, 2H), 2.01 (t, J=2.6Hz, 1H), 1.91 (t, J=6.2Hz, 2H), 1.80-1.73 (m, 2H). 13C NMR (75MHz, CDCl3) delta 158.4, 129.5, 121.1, 114.5, 82.8, 69.2, 62.4, 33.0, 32.7, 26.7, 13.3. Purity: 97.13% by (0.01M KH2PO4 solution: MeOH=15: 85).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-(But-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine, and friends who are interested can also refer to it.

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. 153898-63-6, name is 2-Iodo-5-methoxyaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 153898-63-6

To a solution of 2-iodo-5-methoxy-phenylamine 76a (4.05 g, 16.3 mmole) in [10] ml anhydrous CH2CI2 was added TFAA (4.1 g, 19.5 mmole). The mixture was stirred at [36C] overnight, TLC indicated some starting material remained. Additional TFAA (4.1 g, 19.5 mmole) was added and stirred at [38C] for another 24 hours. The mixture was concentrated under rot vap and purified by column chromatography (eluting with 5-10 % EtOAc in hexanes) to give 4. [6 G] product (81% yield). 1H NMR (300 MHz, [CDCI3) B 7.] 92 [(1 H, D, J= 2.] 8 Hz), 7.66 [(1 H, D, J=] 8.9 Hz), 6.59 (1 H, dd, [J=] 2.8, 8.9 Hz), 3.82 (3H, s).

The synthetic route of 153898-63-6 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. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,2-Dichloro-4-iodobenzene

Thiazolo[5,4-f]quinazolin-9(8H)-one 6 (0.341 mmol), CuI (0.065 g, 0.341 mmol, 1 equiv), and DBU (101 muL, 0.682 mmol, 2.0 equiv) in anhyd DMF (850 muL) were added to a 2 mL glass microwave vial. The mixture was stirred under microwave irradiation at 120 C for 10 min. Then Pd(OAc)2 (7.6 mg, 0.034 mmol, 10 mol%) and the appropriate aryl halide (0.682 mmol, 2.0 equiv) were added to the mixture. The reaction mixture was then stirred under microwave irradiation at 120 C for 5 h. The resulting solution was diluted with CH2Cl2, filtered through a cotton plug and washed with CH2Cl2 (50 mL). The crude product obtained by concentration of CH2Cl2 was purified by flash chromatography on silica gel with EtOAc/CH2Cl2 as eluent (1:0 to 1:1, v/v, for 7ah-j; 7:3 to 1:4, v/v for 7ba-j) to afford the corresponding product 7.

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 20555-91-3.

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. 696-41-3, name is 3-Iodobenzaldehyde, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Iodobenzaldehyde

Reference Example 134 1-(3-iodobenzyl)pyrrolidine To pyrrolidine (0.2 mL) in methanol (10 mL) was added a solution of 3-iodobenzaldehyde (565 mg) in tetrahydrofuran (5 mL), and the mixture was stirred at room temperature for 12 hr. Sodium borohydride (109 mg) was added at 0 C., and the mixture was stirred at room temperature for 2 hr, and concentrated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate. 1 mol/L Hydrochloric acid was added to the extract, and the aqueous layer was washed with ethyl acetate. The obtained aqueous layer was basified with 1 mol/L aqueous sodium hydroxide solution, and the mixture was extracted with ethyl acetate. The extract was washed successively with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound as a yellow oil (382 mg, yield 55%). 1H-NMR (CDCl3) delta: 1.76-1.82 (4H, m), 2.46-2.51 (4H, m), 3.54 (2H, s), 7.03 (1H, t, J=7.5 Hz), 7.27-7.30 (1H, m), 7.55-7.58 (1H, m), 7.69-7.70 (1H, m).

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.