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. 3930-83-4, name is 2-Iodobenzamide, A new synthetic method of this compound is introduced below., name: 2-Iodobenzamide

General procedure: 2-Iodobenzamide 1a (1.0 equiv.), 2-aminoisovaleric acid 2a (3.0 equiv.), Cs2CO3 (3.0 equiv.) and GO/Fe3O4-CuI (Cu+ 0.03 equiv.) were added to DMSO/ethylene glycol (60:1, v/v) in a round bottom flask. The reaction was monitored by TLC. The product was purified by column chromatography with petroleum ether/ethyl acetate (3:1, v/v) to give pure white solid 3a.

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

Application of 83863-33-6,Some common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, molecular formula is C7H8IN, 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.

Production Example 15-1 6-Iodo-1H-indazole An aqueous solution (4 mL) of sodium nitrite (1.1 g) was dropwise added to an acetic acid solution (360 mL) of (5-iodo-2-methylphenyl)amine, and after the addition, this was stirred overnight at room temperature. The solvent was evaporated off under reduced pressure, the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1 to 4:1) to obtain the entitled compound (1 g) as an orange powder.

The synthetic route of 83863-33-6 has been constantly updated, and we look forward to future research findings.

Reference of 49827-15-8, 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. 49827-15-8, name is tert-Butyl 2-iodoacetate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 44 (3.8 g, 1.83 mmol) in anhydrous THF 60 mL under Argon was added NaHMDS (2.2 mL 2.2 mmol, pre-cooled to -78° C.) in THF 30 mL slowly at -78° C. via cannula and the mixture was stirred for 2 min. at -78° C. ICH2CO2tBu (2.35 g, 9.713 mmol) in THF 10 mL was added slowly to the above mixture at -78° C. The dry ice/acetone bath was removed and the stirring was continued for 30 minutes and was poured into NH4Cl aq. solution. The extractive work-up with EA and purification by column chromatography gave 45-1 (upper spot on TLC plate) and 45-2 (lower spot on TLC plate) as two diastereomers about 1:1 mixture (2.9 g, 61percent, combined yield) as yellow oil. 1H NMR (45-1, CDCl3) 7.28-7.22 (9H, m), 6.08 (1H, m), 5.20-5.16 (2H, m), 4.92 (1H, dd, J=2.4 and 8.4 Hz), 4.78 (1H, m), 4.17 (1H, t, J=8.6 Hz), 3.95 (1 H, dd, J=2.7 and 8.8 Hz), 3.35 (1H, t, J=10.0 Hz), 3.15-2.98 (2H, m), 2.75 (1H, dd, J=11.5 and 17.6 Hz), 2.61 (1H, dd, J=3.7 and 17.2 Hz), 1.51 (9H, s), 1.41 (3H, d, J=13.7 Hz), 1.30 (9H, s). 1H NMR (45-2, CDCl3) 7.34-7.15 (9H, m), 6.07 (1H, m), 5.19-5.15 (2 H, m), 4.87 (1H, m), 4.78 (1H, m), 4.05 (1H, t, J=8.4 Hz), 3.96 (1H, m), 3.38 (1H, t, J=9.4 Hz), 3.3.15-3.00 (2H, m), 2.74 (1H, dd, J=11.2 and 17.2 Hz), 2.57 (1H, dd, J=3.9 and 17.4 Hz), 1.51 (9H, s), 1.38 (3H, d, J=13.7 Hz), 1.30 (9H, s).

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, tert-Butyl 2-iodoacetate, other downstream synthetic routes, hurry up and to see.

Some common heterocyclic compound, 160976-02-3, name is 5-Bromo-1,3-difluoro-2-iodobenzene, molecular formula is C6H2BrF2I, 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. COA of Formula: C6H2BrF2I

A 2 M aqueous Na2CO3 solution (1 .51 mL) is added to a mixture of 5-bromo-1 ,3- difluoro-2-iodo-benzene (1 .00 g) and 5-(4,4,5,5-tetramethyl-[1 ,3,2]dioxaborolan-2-yl)- 2-triisopropylsilanyl-oxazole (1 .87 g) in 1 ,4-dioxane (9 mL) and methanol (3 mL). The mixture is sparged with argon and [1 ,1 ‘-bis(diphenylphosphino)-ferrocene]dichloro- palladium dichloromethane complex (380 mg) is added. The resulting mixture is stirred at 80C overnight. Since the conversion is not complete, the same amounts of 5-(4,4,5,5-tetramethyl-[1 ,3,2]dioxaborolan-2-yl)-2-triisopropylsilanyl-oxazole, 2 M aqueous Na2CO3 solution, and catalyst are added and the mixture is again stirred overnight at 80C. The triisopropylsilyl protecting group is cleaved under these conditions. After cooling to room temperature, ethyl acetate and water are added. The aqueous phase is extracted with ethyl acetate and the combined organic phases are washed with brine, dried over MgSO4, and concentrated in vacuo. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 1 :0? 1 :1 ) to afford the title compound. LC (method 4): tR = 1 .18 min; Mass spectrum (ESI+): m/z = 260/262 (Br) [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 160976-02-3, its application will become more common.

Synthetic Route of 19718-49-1, 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. 19718-49-1, name is Methyl 4-amino-3-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(a) 1H-Indole-2,5-dicarboxylic acid 5-methyl ester A solution of 25 g 4-Amino-3-Iodo-benzoic acid methyl ester, 19 ml 2-Oxo-propionic acid, 30.4 g 1,4-Diaza-bicyclo[2.2.2]octane and 1 g Pd(OAc)2 in 200 ml DMF was heated under argon to 100 C. After 5 h the reaction mixture was concentrated under reduced pressure and the residue was partitioned between 300 ml ethyl acetate and 200 ml 1 M hydrochloric acid. The organic layer was dried over MgSO4 and the solvent removed under reduced pressure to yield a yellow solid (6.4 g). From the aqueous layer additional product slowly precipitated as a white solid (7.9 g) which was collected by filtration. Both fractions were combined, dried in vacuo and used in the next reaction without further purification. Yield: 14.3 g. MS (ES+): m/e=220.

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

Application of 355-43-1,Some common heterocyclic compound, 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, molecular formula is C6F13I, 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.

-78 CCooled titanium-dichloride(Cp 2 TiCl 2, 59.8 mg, 0.24 mmol) in ether (2.4 mL)To the solution was added i-propyl magnesium chloride (2.0 M in ether solution, 0.24 mL, 0.48 mmol)1,4-Dioxane (46 [mu] L, 0.54 mmol)And n-tridecafluorohexyl iodide (C 6 F 13 I, 78 muL, 0.36 mmol) were charged, then the temperature was adjusted to -50 C. and stirred for 2 hours.Subsequently, benzaldehyde (20 muL, 0.20 mmol) was added, the temperature was raised, and the mixture was stirred at room temperature for 1 hour.After completion of the reaction, 1 N hydrochloric acid was added to terminate the reaction, followed by extraction with ether three times. The organic layers were combined, dried over sodium sulfate, filtered, and the solvent was distilled off under reduced pressure to obtain a crude product. The obtained crude product was purified by silica gel column chromatography (hexane / ethyl acetate = 20/1 (v / v)) to obtain 2,2,3,3,4,4,5,5,6, 6,7,7,7-tridecafluoro-1-phenyl-1-hydroxyheptane (85.2 mg, yield:> 99%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, its application will become more common.

Some common heterocyclic compound, 7425-53-8, name is Ethyl 4-iodobutanoate, molecular formula is C6H11IO2, 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. Recommanded Product: 7425-53-8

Example 2 1-methyl-3-(carboethoxypropyl)-7-(pivaloyloxymethyl)xanthine A mixture of 1-methyl-7-(pivaloyloxymethyl)xanthine (350mg, 1.25 mmes) sodium carbonate (265mg, 2.50 mmoles) and ethyl 4-iodobutyrate (384 mul, 2.50 mmole) in 5.8ml dry DMF was stirred under nitrogen at room temperature for 18 hours. Water was added and the reaction mixture extracted with chloroform. After drying, the extracts were stripped to leave a yellow oil which goes to chromatographed on four thick silica gel plates with 10% EtOH/CHCl3. The band was scraped off and eluted with 100ml of 25% EtOH/CHCl3 to yield 609mg of the desired product as an oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 7425-53-8, its application will become more common.

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. 13194-68-8, name is 4-Iodo-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

(b) Preparation of 5-Bromo-3,4-difluoro-2-(4-iodo-2-methyl-phenylamino)-benzoic acid To a stirred solution comprised of 1.88 g (0.00791 mol) of 2-amino-5-iodotoluene in 10 mL of tetrahydrofuran at -78 C. was added 6 mL (0.012 mol) of a 2.0 M lithium diisopropylamide in tetrahydrofuran/heptane/ethylbenzene (Aldrich) solution. The resulting green suspension was stirred vigorously for 10 minutes, after which time a solution of 1.00 g (0.00392 mol) of 5-bromo-2,3,4-trifluorobenzoic acid in 15 mL of tetrahydrofuran was added. The cold bath was subsequently removed, and the reaction mixture stirred for 18 hours. The mixture was concentrated, and the concentrate was treated with 100 mL of dilute (10%) aqueous hydrochloric acid. The resulting suspension was extracted with ether (2*150 mL), and the combined organic extractions were dried (MgSO4) and concentrated in vacuo to give an orange solid. The solid was triturated with boiling dichloromethane, cooled to ambient temperature, and collected by filtration. The solid was rinsed with dichloromethane, and dried in the vacuum-oven (80 C.) to afford 1.39 g (76%) of a yellow-green powder; mp 259.5-262 C.; 1H NMR (400 MHz, DMSO): delta9.03 (s, 1H), 7.99 (dd, 1H, J=7.5, 1.9 Hz), 7.57 (dd, 1H, J=1.5 Hz), 7.42 (dd, 1H, J=8.4, 1.9 Hz), 6.70 (dd, 1H, J=8.4, 6.0 Hz), 2.24 (s, 3H); 19F NMR (376 MHz, DMSO): delta-123.40 to -123.47 (m); -139.00 to -139.14 (m); IR (KBr) 1667 (C=O stretch)cm-1; MS (CI) M+1=469. Analysis calculated for C14H9BrF2INO2: C, 35.93; H, 1.94; N, 2.99; Br, 17.07; F, 8.12; I, 27.11. Found: C, 36.15; H, 1.91; N, 2.70; Br, 16.40; F, 8.46; I, 26.05.

According to the analysis of related databases, 13194-68-8, the application of this compound in the production field has become more and more popular.

Electric Literature of 101335-11-9, A common heterocyclic compound, 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, molecular formula is C6H3ClFI, 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 mixture of 8-{[tert-butyl(dimethyl)silyl]oxy}-3-methyl-2-azaspiro[4.5]decan-1 -one (mixtureof isomers) (329 mg, 1.11 mmol) and 2-chloro-4-fluoro-1-iodobenzene (340 mg, 1.33 mmol)in o-xylol (20 ml) was added under an argon atmosphere copper(l) iodide (42.1 mg, 221 pmol), N,N?-imethylethylenediamine (48 p1, 440 pmol) and potassium phosphate (469 mg,2.21 mmol) and the reaction was heated to 1400 for 24 h in a microwave reactor. Upon cooling, the reaction mixture was filtrated through a pad of celite the residue was washedwith ethyl acetate and the filtrate was concentrated under reduced pressure. The crude product was purified by flash chromatography (hexanes/ethyl acetate-gradient, 0% -> 10% ethyl acetate) to give the title compound (280 mg).[C-MS (Method 2): R = 1.75 mm; MS (ESIpos): m/z = 426 [M+H]+ 1H-NMR (400 MHz, DMSO-d6): 6 [ppm] = 7.55 (dd, 1H), 7.44-7.33 (m, 1H), 7.31-7.16 (m,1H), 4.06-3.97 (m, 1H), 3.94-3.85 (m, 1H), 2.12-1.98 (m, 1H), 1.92-1.76 (m, 1H), 1.71 -1 .36(m, 6H), 1.26-1.14(m, 1H), 0.98(d, 3H), 0.88-0.80(m, 9H), 0.01 (d, 6H)

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: 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, 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 52548-63-7, Safety of 5-Fluoro-2-iodobenzoic acid

To a solution of 5-fluoro-2- iodo-benzoic acid (3.86 g, 14.65 mmol), 2H-[1 ,2,3]triazole (2.5 g, 36.2 mmol), CS2CO3 (8.62 g, 24.5 mmol), trans-N, N’-dimethyl-cyclohexane-1 ,2-diamine (0.4 ml_), Cul (244 mg) and DMF (13 ml_) were added to a microwave ready vessel and heated to 100oC for 10 min. The mixture was cooled, diluted with water, and extracted with EtOAc. The aqueous layer was acidified and extracted with EtOAc. The organic layer was dried over Na2SO4 and concentrated.Chromatography (DCM to 10% MeOH/1 % HOAc/DCM) gave the product as a white powder (2.14 g, 71 %). 1H NMR (400 MHz, CD3OD): 7.91 (s, 2H), 7.76 (dd, J = 8.9, 4.8 Hz, 1 H), 7.59 (dd, J = 8.5, 2.9 Hz, 1 H), 7.49 – 7.42 (m, 1 H).

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.