Tag: M.W=300-400

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. 31928-47-9, name is 4-Bromo-2-chloro-1-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H3BrClI

A mixture of Xantphos (1.20 g, 2.05 mmol) and tris(dibenzylideneacetone)dipalladium (0) (1.26 g, 1.37 mmol) in anhydrous anisole (76 mL) was stirred under nitrogen, at 50 0C for 30 minutes to provide a an orange- brown solution of the catalyst.[00326] To a stirred mixture of 6-amino-7-fluoro-3-methyl-3H-benzoimidazole-5- carboxylic acid methyl ester (6) (8.00 g, 34.16 mmol) and cesium carbonate (22.48 g, 68.31 mmol) in anhydrous anisole (76 mL) under nitrogen was added 4-bromo-2- chloroiodobenzene (1.60 g, 1.10 equiv., 4.88 mmol). The preformed catalyst, as prepared above, was then added to the mixture to provide a dark brown suspension, which was heated at 100 +/- 2 0C, with stirring at 350 rpm. The reaction was monitored by HPLC analysis. After 41 hours, no 6-amino-7-fluoro-3-methyl-3//-benzoimidazole-5-carboxylic acid methyl ester (6) remained. The reaction mixture was cooled to about 80 0C and IM sulfuric acid (40.99 mL 40.99 mmol) was added. Gas evolution was observed after 10 minutes and the rate of addition was controlled to moderate the effervescence. At the end of the addition the pH was between 7 and 8. Additional sulfuric acid (IM, 10.25 mL, 10.25 mmol) was then added to give mobile slurry with a pH of 0. The mixture was diluted with anisole (20 mL) and Celatom FW- 14 filter agent was added. It was then filtered at about 80 C through a water-wet pad of Celatom FW- 14 filter agent and the cake was washed with anisole (1 x 40 mL + 3 x 20 mL), then water (10 mL). The lower aqueous layer was separated and discarded and the organic layer was washed with 10 % aqueous NaCl solution (2 x 40 mL). This was added to a sodium hydroxide (5.46 g, 68.3 mmol) in methanol (24 mL) and the mixture was heated at 65 C with stirring. After 17.5 hours HPLC analysis indicated that the hydrolysis of the ester was complete and the slurry was cooled to 15 C, then filtered on a sinter. The solid was washed with water (4 x 24 mL), MTBE (24 mL), and acetonitrile (2 x 25 mL) and then dried at 45 0C in a vacuum oven to provide 11.07 g of 6-(4- EPO bromo-2-chlorophenylamino)-7-fluoro-3-methyl-3H-benzoimidazole-5-carboxylic acid (7) as a fine pale brown solid (assay 93.7% by 1H NMR), actual wt 10.37 g (72.2% yield). 1H NMR (400 MHz, d6 DMSO) delta 3.85 (3H, s, NMe), 6.53 (IH, dd, J 9, 7, Ar-H), 7.27 (IH, dd, J 9S 2.5, Ar-H), 7.56 (IH, d, J 9, Ar-H), 7.97 (IH, s, Ar-H), 8.20 (IH5 s, Ar-H), 11.5 (IH, s, CO2H). 13C NMR (100 MHz, d6 DMSO) delta 31 (CH3), 108 (CH, d, J 2), 109 (CH), 117 (C, d, J6), 122 (C), 124 (C, d, J7), 127 (C)5 130 (C)5 131 (C), 132 (C, d, J9), 133 (C5 d, J l l), 141 (C), 145 (CF, d5 J 252), 146 (CH)5 170 (C=O).

According to the analysis of related databases, 31928-47-9, the application of this compound in the production field has become more and more popular.

Electric Literature of 98-61-3, 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. 98-61-3, name is 4-Iodobenzenesulfonyl chloride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

5.1.16 4-((4-Iodophenylsulfonamido)methyl)-N-(pyridin-3-yl)benzamide (28) A mixture of amine 27 (727 mg, 3.2 mmol) and 4-iodobenzenesulfonyl chloride (970 mg, 3.2 mmol) in dry pyridine (10 mL) was stirred at 20 C for 16 h. The solvent was evaporated and the residue stirred in water (20 mL) for 1 h. The precipitate was filtered, washed with water (5 mL) and dried. The crude solid was purified by column chromatography, eluting with a gradient (0-20%) of MeOH/EtOAc, to give benzamide 28 (1.47 g, 93%) as a cream powder: mp (MeOH/EtOAc) 249-251 C; 1H NMR delta 10.36 (s, 1H, NHCO), 8.93 (d, J = 2.3 Hz, 1H, H-2′), 8.34 (br s, 1H, NHSO2), 8.31 (dd, J = 4.7, 1.5 Hz, 1H, H-6′), 8.18 (ddd, J = 8.3, 2.5, 1.5 Hz, 1H, H-4′), 7.97 (ddd, J = 8.6, 2.2, 1.9 Hz, 2H, H-2″, H-6″), 7.90 (br d, J = 8.3 Hz, 2H, H-2, H-6), 7.56 (ddd, J = 8.6, 2.2, 1.9 Hz, 2H, H-3″, H-5″), 7.37-7.42 (m, 3H, H-3, H-5, H-5′), 4.09 (s, 2H, CH2N); 13C NMR delta 165.5, 144.5, 142.0, 141.6, 140.3, 138.1 (2), 135.8, 133.1, 128.2 (2), 127.7 (2), 127.5 (2), 127.3, 123.5, 100.3, 45.7; MS m/z 494.6 (MH+, 100%). Anal. Calcd for C19H16IN3O3S: C, 46.26; H, 3.27; N, 8.52. Found: C, 46.43; H, 3.30; N, 8.52.

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

Electric Literature of 391211-97-5, These common heterocyclic compound, 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, 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 an oven-dried three-neck, 2 L flask was taken 3, 4-DUFLUORO-2- [ (2- fluoro-4-iodophenyl) amino] benzoic acid (196.7g, 0.5 moles) and DMF (900 mL). To this stirred solution was added pyridine (44.4 mL, 43.5g, 0.55 moles) at RT, and then pentafluorophenyl trifluoroacetate (95 mL, 154g, 0.55 moles) was added dropwise within 30 minutes. The mixture was stirred at RT for 20 hours. The mixture was diluted with hexanes-diethyl ether (1 : 1, v/v, 3L) and washed successively with water (2x2L), 1M HC1 (2x2L), saturated NAHCO3 solution (2x2L) and finally with water (2x2L). The organic layer was dried and concentrated under reduced pressure to afford 2,3, 4,5, 6-pentafluorophenyl-3,4- difluoro-2- [ (2-fluoro-4-iodophenyl) amino] benzoate as a red oil (92.3%, 258.5g).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.

Related Products of 34270-90-1, A common heterocyclic compound, 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, molecular formula is C4H8I2O, 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.

Spiro[4H-pyran-4,10′(4’H)-[6H]pyrimido[2,1-c][1,4]thiazepine]-2′-carboxylic acid, 2,3,5,6,7′,8′-hexahydro-3′-hydroxy-4′-oxo-, ethyl ester, 9′,9′-dioxide: To a stirred yellow mixture of intermediate 19/24 (0.1942 g, 0.50 mmol) intermediate 18 (0.208 g, 0.62 mmol) in DMF (5 mL) wad added Cs2CO3 (0.332 g, 1.02 mmol) at once at room temperature. After 24 h, the reaction mixture was diluted with Et2O (50 mL), washed with water (2×10 mL), brine (10 mL), dried (Na2SO4), filtered and concentrated to give colorless paste which was used in the subsequent step without purification.

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.

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. 628-21-7, name is 1,4-Diiodobutane, A new synthetic method of this compound is introduced below., COA of Formula: C4H8I2

A12 (50.0 mg, 244.82 mumol), 1,4-diiodobutane (48 muL, 367.23 mumol), potassium carbonate (50.8 mg, 367.23 mumol), and anhydrous N, N-dimethylformamide (3 mL) It was added to a 10 mL eggplan60t-shaped flask and stirred at 60 C for 4 hours. After the reaction was detected by TLC, it was filtered and the filtrate was concentrated. After recrystallization (petroleum ether / ethyl acetate, volume ratio of 1: 1), 60.0 mg of white solid was obtained with a yield of 95%. mp: 100-102 C;

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 16355-92-3, name is 1,10-Diiododecane, 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 16355-92-3, Formula: C10H20I2

2,15-hexadecanedione as an aliphatic diketone was synthesized. In a 2 L four-necked flask equipped with a thermometer, mixer and a reflux condenser, 260.3 g (2.0 mol) of ethyl acetoacetate and 500 ml of acetone were fed, stirred and mixed, 61.9 g (1.5 mol) of 97% sodium hydroxide was added and reacted for 15 minutes. Then 197.0 g (0.5 mol) of 1,10-diiododecane was added and the reaction was carried out under reflux for 6 hours. After completion of the reaction, acetone was distilled off by distillation under reduced pressure, neutralized by adding 2N hydrochloric acid, and separation was carried out. The upper layer organic layer was separated and 800 g (2.0 mol) of 10% sodium hydroxide aqueous solution was added and stirred at room temperature for 8 hours to carry out a saponification reaction, 205.8 g (1.1 mol) of 50% sulfuric acid was added, and the mixture was fully refluxed for 3 hours for decarboxylation reaction. After the decarboxylation reaction was completed, the upper organic layer was separated by phase separation and cooled to room temperature to obtain 130.8 g of a pale yellow crystal. A small amount of a part of the obtained crystal product was taken for gas chromatograph measurement. As a result of analyzing the composition of the separated crystals by gas chromatography, the conversion of 1,10-diiododecane was 100%, the purity of 2,15-hexadecanedione was 92%.The yield of 2,15-hexadecanedione based on 1,10-diiododecane was 95%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,10-Diiododecane, and friends who are interested can also refer to it.

Synthetic Route of 1271523-34-2, A common heterocyclic compound, 1271523-34-2, name is 1,5-Dichloro-2-iodo-3-methoxybenzene, molecular formula is C7H5Cl2IO, 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 solution of 11a (21.0g, 69.3mmol) in THF (250ml) was sequentially added Cul (1.32g, 6.9mmol) and NaH (60% dispersion in mineral oil, 4.2g, 104mmol), followed by a slow addition of pinacolborane (15.1ml, 104mmol). The resulting suspension was stirred at room temperature for 16 h under a N2 atmosphere, and then quenched with saturated NH4CI (250 ml). After 20 min, the mixture was extracted with EtOAc (x3), dried and then filtered over Celite. Concentrated and purification by column chromatography (Si02; EtOAc:PE 0: 1?3:7) to afford the title boronate as a white solid; (15. lg, 72%)NMR (CDC13) 6.87 (IH, d, J 1.6), 6.63 (IH, d, J 1.6), 3.37 (3H, s), 1.32 (12H, s);MS (m/e) No MI observed, Rt 1.17min (QC Method 2)

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 181765-86-6, A common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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.

Example 5 [00619] Preparation of Cpd 30 [00620] Step A: A mixture of methyl 5-bromo-2-iodobenzoate (18.4 g, 54.0 mmol), TMS acetylene (8.5 mL, 5.88 g, 60.0 mmol), Cul (0.51 g, 2.7 mmol), PdCl2(Ph3P)2 (1.9 g, 2.7 mmol), Et3N (15.0 mL, 10.9 g, 108.0 mmol) and acetonitrile (100 mL) was stirred under argon at room temperature for 4 hours. After the removal of the volatiles in vacuo, the residue was chromatographed (silica gel, ethyl acetate in hexanes, 0-20%) to provide the TMS alkyne intermediate as colorless oil (15.7 g, 94%).

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: 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, 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 199786-58-8, Computed Properties of C7H6BrIO

To a stirred solution of PDC (11.0 g, 0.0288 mol) in CH2Cl2 (60 mL) was added a solution of 11 (4.50 g, 0.0144 mol) in CH2Cl2 (20 mL). The mixed content was stirred for 4 h at rt. The solvent was then removed under vacuum to give the crude product of 12, which was purified by silica flash column chromatography (hexanes/CH2Cl2, 7:3) to give compound 12 (4.40 g, 0.0142 mol, 98%) as a white solid.

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.

Related Products of 21740-00-1,Some common heterocyclic compound, 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, molecular formula is C7H4BrIO2, 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.

A mixture of 5-bromo-2-iodobenzoic acid (2) (800 mg, 2.447 mmol) and 3.5 mL of thionyl chloride was refluxed with stirring for 1 h under a N2 atmosphere, then excess of thionyl chloride was removed in vacuo. Under N2 atmosphere, sodium azide (191 mg, 2.9 mmol) and dry acetone (7 mL) were poured into the flask containing the crude acyl chloride and the mixture was stirred at room temperature for 10 min, after that, acetone was removed in vacuo. CAUTION, the acyl azide is potentially explosive, the solution should not be evaporated to complete dryness. The residue was dissolved in dry toluene (7 mL) and the mixture was stirred at 80-85 C for 3.5 h under a N2 atmosphere. To the reaction flask was added benzyl alcohol (258.0 muL, 2.5 mmol) and 4-dimethylaminopyridine (DMAP, 7.5 mg, 0.06 mmol), the resulting mixture was again stirred at 80-85 C for 1 h under N2 atmosphere. The reaction mixture was diluted with ethyl acetate and after the usual aqueous work up, the organic layer was concentrated to yield a solid residue. This solid was dissolved in dichloromethane and then petroleum ether was added to precipitate the product which was triturated and washed with dichloromethane/petroleum ether mixture to afford (3) 861 mg, 81% yield.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Bromo-2-iodobenzoic acid, its application will become more common.