Tag: M.W=200-300

Related Products of 13194-68-8, A common heterocyclic compound, 13194-68-8, name is 4-Iodo-2-methylaniline, molecular formula is C7H8IN, 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.

4-iodo-2-methylbenzenamine 24 (233 mg, 1 mmol) on reaction with 1-tert-butyl-4-ethynylbenzene (25b, 158 mg, 1 mmol) by employing Sonagashira coupling conditions using Pd(PPh3)4 (69.3 mg, 0.06 equiv) as catalyst, Cul (22.8 mg, 0.12 equiv) as cocatalyst, butyl amine (261 mg, 3 equiv) as base and ether as solvent and kept the reaction for 6 h. After completion of the reaction as indicated by TLC and the reaction mixture is extracted into ether (4×25 mL) from the aqueous layer and concentrated in vacuo. The compound was further purified by column chromatography using 60-120 silica gel (ethyl acetate/hexane,1:9) to obtain 4-((4-tert-butylphenyl) ethynyl)-2-methyl benzene amine (26b) as pure product. Anthranilic acid (27, 137 mg, lmmol) on reaction with acetic anhydride at 150 C. and reflux for 30 min, after completion of reaction aqueous sodium bicarbonate solution is added and extracted in ethyl acetate (4×25 mL) from the aqueous layer and concentrated in vacuo afforded 2-methyl 4H-benzo[d][1,3]oxazin-4-one compound ( 28) as pure product. To a stirred solution of 4-((4-tertbutylphenyl)ethynyl)-2-methylbenzenamine (26b, 263 mg, 1 mmol) with 2-methyl-4H-benzo[d][1,3]oxazin-4-one (28, 161 mg, 1 mmol) in acetic acid and reflux for 8 h After completion of the reaction as indicated by TLC. then the reaction mixture was quenched with NaHCO3 and extracted in ethyl acetate (4×25 mL) from the ice cold aqueous layer and dried over anhydrous Na2SO4 afforded 3-(4-((4-tert-butylphenyl)ethynyl)-2-methylphenyl)-2-methylquinazolin-4(3H)-one (29b). Reaction of 3-(4-((4-tert-butylphenyl)ethynyl)-2-methylphenyl)-2-methylquinazolin-4(3H)-one (29b, 406 mg, 1 mmol) with 2,4-dihydroxybenzaldehyde (30d, 138 mg, 1 mmol) was taken in acetic acid Then the resulting mixture was stirred under reflux conditions for 8 h and then the reaction mixture was quenched with NaHCO3 and extracted in ethyl acetate (4×25 mL) from the ice cold aqueous layer and dried over anhydrous Na2SO4.The resulting product ( 5d) was purified by column chromatography employing EtOAc/Hexane as an eluent.

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.

Synthetic Route of 6828-35-9, 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. 6828-35-9 name is 5-Chloro-2-iodoaniline, 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.

5-Chloro-2-((trimethylsilyl)ethynyl)aniline To a solution of 5-chloro-2-iodoaniline (1.50 g, 5.92 mmol) and ethynyltrimethylsilane (1.25 ml, 8.88 mmol) in Et3N (20 ml) was added CuI (5.6 mg, 0.030 mmol) and Pd(PPh3)2Cl2 (21 mg, 0.030 mmol) and the mixture was stirred at room temperature for 5 hours. Celite was added and the suspension was filtered, rinsed with EtOAc. The filtrate was concentrated in vacuo to yield Intermediate 1 as a yellow oil (1.32 g, 100%). 1H NMR (CHLOROFORM-d) delta: 7.20 (d, J=8.2 Hz, 1H), 6.69 (d, J=1.8 Hz, 1H), 6.63 (dd, J=8.2, 2.1 Hz, 1H), 4.30 (br. s., 2H), 0.27 (s, 9H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Chloro-2-iodoaniline, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane, 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 461-17-6, Recommanded Product: 461-17-6

Step 1. Preparation of tert-butvl fM-(4.4,4-trifluorobutvl)piperidin-3-vnmethvl)carbamate; O CH3T rcH3O CH3[122] To a mixture of tert-butyl (piperidin-3-ylmethyl)carbamate (0.30 g, 1.40 mmol) in anhydrousCH3CN (10 ml_) was added CsF-celite (0.53 g) followed by 1-iodo-4,4,4-trifluorobutane (0.40 g,1.68 mmol). The mixture was heated to reflux and stirred for 16 h. The mixture was diluted withEtOAc, filtered through a pad of Celite and then concentrated to dryness under reducedpressure. Water (40 ml_) was added, and the mixture was extracted with CH2CI2 (2 x 40 mL) andEtOAc (1 x 40 mL). The combined organic layers were dried over MgSO4, filtered, andconcentrated in vacuo. The white residue was taken up in CH2CI2 (with a minimal amount ofMeOH) and loaded onto a silica gel column. The mixture was then purified by silica gel flashchromatography (97% CH2CI2: 3% 2M NH3 in MeOH). This gave the product as a light yellow oil(0.31 mg, 68%). 1H NMR (300 MHz, CD3CN) 8 5.30 (br s, 1H), 2.86-2.90 (m, 2H), 2.66-2.73 (m,2H), 2.29-2.34 (m, 2H), 2.09-2.23 (m, 2H), 1.95-1.99 (m, 2H), 1.57-1.71 (m, 6H), 1.37 (s, 9H),0.83-0.99 (m, 1H); ES-MS m/z325.1 (MH+); HPLC RT (min) 1.76.

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, 1,1,1-Trifluoro-4-iodobutane, other downstream synthetic routes, hurry up and to see.

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 627-31-6 as follows. Quality Control of 1,3-Diiodopropane(stabilized with Copper chip)

The beta- lactam carbonyl compound shown in the formula CH3CH2-COCH2CONH-C6H4Cl1.0mmol added 50 ml round-bottomed flask, and then sequentially adding K2CO32.4mmol, 0.10 mmol tetrabutylammonium chloride, ammonium acetate 1.1mmol, 1,3Diiodopropane 1.2mmol and 35mL of deionized water and mix well. The reaction was continued stirring at 20 10.0 hours, the reaction was stopped by filtration, dried and purified by recrystallization after give 6- (4-chloro-anilino) -5-propionyl-3,4-dihydropyran, products yield 96%.

According to the analysis of related databases, 627-31-6, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, molecular formula is C9H9IO2, 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. Application In Synthesis of Methyl 3-iodo-4-methylbenzoate

A mixture of methyl 3-iodo-4-methylbenzoate (1.0 g, 3.6 mmol) and CuCN (389 mg, 4.3 mmol) in NMP (10 mL) is stirred at 200 oC for 1 hour with microwave irradiation.The mixture is diluted with EtOAc / toluene (10:1, 50 mL) to afford precipitate, which is separated by filtration through a pad of Celite. The filtrate is washed with water (30 mL x 3), brine (20 mL x 1), dried over sodium sulfate.The insoluble materials are separated by filtration and the filtrate is concentrated.The residue is purified by column chromatography on silica-gel eluting with n-hexane / EtOAc (7:1 to 6:1) to give 511 g (81% yield) of the title compound as a white solid. 1H-NMR (400 MHz, CDCl 3) delta8.27 (1H, d, J = 1.8 Hz), 8.13 (1H, dd, J = 8.6, 1.8 Hz), 7.42 (1H, d, J = 8.6 Hz), 3.94 (3H, s), 2.61 (3H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 90347-66-3, its application will become more common.

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 573764-31-5 as follows. name: 4-Chloro-3-iodoaniline

General procedure: A mixture of compound 3 (5 mmol), phenylboronic acid (10 mmol), Pd(Ph3P)4 (0.1 mmol), Na2CO3 (10 mmol) in 1,4-dioxane/H2O (20 mL) was stirred at 110 °C for 24 h under Ar. The reaction mixture was filtered through celite. The filtrate was concentrated in vacuo and then extracted with EtOAc. The organic layer was evaporated to give a residue, which was purified by chromatography (petroleum ether/EtOAc, 10:1) to give pure product as a yellow liquid, yield 88percent.

According to the analysis of related databases, 573764-31-5, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 33994-44-4, name is Methyl 3-(4-Iodophenyl)propanoate, 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 33994-44-4, name: Methyl 3-(4-Iodophenyl)propanoate

A 500 ml three-neck flask is charged with 14.0 g of 4-(2-thienyl)acetoanilide, 22.4 g of methyl 4-iodophenylpropionate, 13.4 g of potassium carbonate, 0.8 g of copper sulfate pentahydrate and 40 ml of o-dichlorobenzene, and the mixture is stirred under heating at 200 C. for 15 hours in a nitrogen stream. After this reaction, 100 ml of ethylene glycol and 5.4 g of potassium hydroxide are added to the reaction mixture, which is then refluxed under heating for 3 hours in a nitrogen stream, then cooled to ambient temperature, poured into 300 ml of distilled water and neutralized by hydrochloric acid to thereby precipitate crystals. The crystals are filtered, sufficiently washed with water and then transferred to a 1 L flask. To the crystals is added 500 ml of toluene, followed by refluxing under heating to remove water by azeotropic distillation. Then, 100 ml of methanol and 1 ml of concentrated sulfuric acid are added thereto, and the resulting mixture is refluxed under heating for 2 hours in a nitrogen stream. After the reaction, the reaction solution is dissolved in distilled water and extracted with toluene. The organic phase is sufficiently washed with distilled water. Next, the organic phase is dried by sodium sulfate anhydride, a solvent is evaporated off under reduced pressure and the residue is recrystallized from an ethyl acetate-hexane mixed solution to thereby obtain 15.1 g of diarylamine. A 100 ml flask is charged with 5.5 g of the thus-obtained diarylamine, 3.2 g of 4,4-diiodobiphenyl, 2.2 g of potassium carbonate, 0.2 g of copper sulfate pentahydrate and 10 ml of o-dichlorobenzene, and the mixture is refluxed under heating for 9.5 hours in a nitrogen stream. After the reaction is completed, the reaction mixture is cooled to ambient temperature and dissolved in 100 ml of toluene, and unnecessary substances are removed by filtration. An obtained filtrate is purified by silica gel column chromatography using toluene, to thereby yield 6.2 g of a thiophene-containing compound (Exemplary Compound 7). A melting point of the resulting thiophene-containing compound is 110 to 112 C. The IR spectrum (obtained using a KBr tablet method) of the thiophene-containing compound is shown in FIG. 2. An 1H-NMR spectrum (in a CDCl3 solvent) of the thiophene-containing compound is shown in FIG. 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, Methyl 3-(4-Iodophenyl)propanoate, other downstream synthetic routes, hurry up and to see.

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 916792-62-6 as follows. Formula: C7H3FIN

Intermediate 50: 3-Fluoro-2-(pyrimidin-2-yl)benzoic acid.Step A: 3-Fluoro-2-(pyrimidin-2-yl)benzonitrile. 2-lodo-3- fluorobenzonitrile (2.5 g, 10.3 mmol) and 2-tributylstannane pyrimidine (3.7g, 10.0 mmol) were combined and dissolved in degassed DME (18 ml) then purged with bubbling N2 for 5 minutes. The reaction was treated withPd(PPh3)4 (577 mg, 0.5 mmol) and then purged with bubbling for 5 minutes in a sealed vessel and then heated in microwave at 160 C for 90 min. The reaction was cooled and filtered through celite and concentrated to minimum volume and the ppt the formed was diluted with hexanes (40 ml) and cooled to 0 C then filtered. The solid purified (FCC) (20-100% EA / hex) to give 3-fluoro- 2-(pyrimidin-2-yl)benzonitrile. 1 H NMR (400 MHz, CDCI3): 8.93 (d, J = 4.9 Hz, 2H), 8.14 (dd, J = 9.6, 2.7 Hz, 1 H), 7.86 (dd, J = 8.6, 5.3 Hz, 1 H), 7.36 (t, J = 4.9 Hz, 1 H), 7.32 – 7.24 (m, 1 H).

According to the analysis of related databases, 916792-62-6, the application of this compound in the production field has become more and more popular.

Electric Literature of 620621-48-9, A common heterocyclic compound, 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, molecular formula is C8H6ClIO2, 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.

8.1 2-Chloro-5-(pyrimidin-4-ylamino)-benzoic acid methyl ester Sodium phenoxide (810 mg), tris(dibenzylideneacetone)dipalladium (0) (102 mg), Xantphos (161 mg) and methyl-2-chloro-5-iodobenzoate (1379 mg) were placed in a flask and flushed with argon. 4-aminopyrimidine (486 mg) and dioxane (27.5 mL) were added and the reaction mixture was heated to 120 C. for 18 h. After cooling to RT, it was diluted with EtOAc and washed with a 1M solution of NaOH. The organic phase was dried over MgSO4 and concentrated in vacuo. The crude material was purified by CC (Hept/EtOAc 1/1 to 0/1) to give 718 mg of the titled compound as a yellowish powder. LC-MS (B): tR=0.48 min; [M+H]+: 264.21.

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. 146137-72-6, name is 2-Fluoro-6-iodobenzaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H4FIO

Step 2: To a solution of 2-fluoro-6-iodobenzaldehyde (1.5 g, 6.0 mmol) and 2-bromopyridine-3, 4- diamine (1.1 g, 6.0 mmol) in ethanol (20 mL), was added ferric chloride (778 mg, 4.80 mmol). The reaction mixture was stirred at 60 C under oxygen atmosphere overnight. The next day, solvent was evaporated via rotavap and theresulting residue was purified by column chromatography on silica gel eluting with petroleum/ethyl acetate (3 :1) to give the desired product (1.6 g, 64% yield) as a yellow solid. LCMS (ESI) m/z: 418 [M+H+].

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 146137-72-6.