Month: April 2021

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. 825-98-9, name is 3-Fluoro-4-iodobenzoic acid, A new synthetic method of this compound is introduced below., name: 3-Fluoro-4-iodobenzoic acid

To a solution of 3-fluoro-4-iodobenzoic acid (step-iof Intermediate-27, i.0 g, 3.75 mmol) inDMF (iO mL) was added K2C03 (i.07 g, 7.5i mmol), 2-bromo-N,N-diethylacetamide (i.09 g,5.63 mmol).The reaction mass was stirred at 80-90C for i6 h. The reaction mixture wasquenched with water, extracted with DCM. The organic layers were dried over Na2504 and concentrated to afford 0.500 g of title compound. ?H NMR (300 MHz, DMSO-d6): 8.09- 8.04 (t, J = 6.6 Hz, iH), 7.73-7.70 (t, J = 8.i Hz, iH), 7.60-7.57 (t, J = 7.8 Hz, iH), 5.03 (s, 2H), 3.30-3.i9 (q, J= 7.5 Hz, 4H), i.i7-i.i3 (t, J= 7.5 Hz, 3H), i.04-0.99 (t, J= 7.2 Hz, 3H);MS [M+Hf?: 380.

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: 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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 627-31-6, COA of Formula: C3H6I2

In a 25 mL flask, xanthene (1, 350 mg, 1.92 mmol),dissolved in dry THF (10 mL) and diiodopropane (0.2 mL 1.74 mmol) were stirred under argon at 0 C. n-Butyllithium (1 mL, solution 2.5 M in hexanes) was added dropwise, after which the reactionwas heated up to room temperature. After approx 2 h (TLC 40% hexane-CHCl3 7:3), solvent was evaporated in vacuo. The crude product was dissolved in DCM (75 mL), washed three times withwater (30 mL), dried over Na2SO4 and taken to dryness in vacuo. The crude product was purified byflash column chromatography (0%-40% CHCl3 in hexane), to give 12 as a white powder, (410 mg,0.93 mmol, 48% yield).

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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Synthetic Route of 128140-82-9, A common heterocyclic compound, 128140-82-9, name is 1-(Difluoromethoxy)-4-iodobenzene, molecular formula is C7H5F2IO, 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.

[0712] Compound 655 was prepared following the similar procedure described in the synthesis of compound 593 where 1-(difluoromethoxy)-4-iodobenzene was used in place of XIII-10, and CuI Cs2CO3, and 8-hydroxyquinoline in DMSO/dioxane used as the reaction catalysts. The reaction mixture was purged with N2 and stirred at 110 C. overnight. In the last step coupling reaction, Pd-118 and K3PO4 were used in place of Pd(dppf)Cl2 and K2CO3. 1H NMR (DMSO-d6, 400 MHz) delta 8.10 (s, 1H), 7.79 (s, 1H), 7.54-7.51 (m, 3H), 7.32-7.14 (m, 4H), 6.59 (d, J=2.8 Hz, 1H), 4.51 (q, J=7.2 Hz, 2H), 3.85 (s, 3H), 1.33 (t, J=7.2 Hz, 3H).

The synthetic route of 128140-82-9 has been constantly updated, and we look forward to future research findings.

Related Products of 68507-19-7,Some common heterocyclic compound, 68507-19-7, name is 3-Iodo-4-methoxybenzoic acid, molecular formula is C8H7IO3, 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 9. (3 -Difluoro-5-(5-methyl-[l ,2,41triazolo[l ,5-alpyrimidin-7-yl)piperidin- l-yl)(3-iodo-4-methoxy hen l)methanone. To a solution of 7-(5,5-difluoropiperidin-3-yl)-5-methyl-[l ,2,4]triazolo[l,5- a]pyrimidine (35 mg, 0.10 mmol) in DCM (0.32 mL) was added TEA (15.94 mu, 0.1 1 mmol), 3-iodo-4-methoxybenzoic acid (26.50 mg, 0.10 mmol), HOBt (17.51 mg, 0.1 1 mmol) and EDCI (21.92 mg, 0.1 1 mmol). The reaction was stirred at rt for 16 h. The crude reaction was filtered and the residue was purified by preparative reverse phase HPLC to afford the title compound (14 mg, 29%). 1H NMR (400 MHz, CDC13) delta = 8.58 (s, 1H), 7.95 (d, J = 1.96 Hz, 1H), 7.50 (dd, J = 8.41 , 2.15 Hz, 1H), 6.94 (br s, 1H), 6.86 (d, J = 8.61 Hz, 1H), 4.52 – 4.85 (m, 1H), 4.03 (br s, 2H), 3.88 – 3.99 (m, 3H), 3.23 – 3.58 (m, 2H), 2.65 – 2.76 (m, 5H), [M+H] = 514.1.

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-4-methoxybenzoic acid, its application will become more common.

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.

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. 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.

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.

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.

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.