Tag: M.W=200-300

Synthetic Route of 42048-11-3, 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. 42048-11-3, name is 2-Chloro-6-iodotoluene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Palladium acetate palladium (44.9 mg, 0.2 mmol) was added to a 25 mL eggplant bottle.Triphenylphosphine (52.4 mg, 0.2 mmol),Sodium formate (276 mg, 4 mmol),Norbornene (188 mg, 2 mmol),Potassium phosphate (2.544 g, 12 mmol),Potassium acetate (392 mg, 4 mmol),2-chloro-6-sulfonic acid toluene (504 mg, 2 mmol),Ethyl bromobutyrate (1.56 g, 8 mmol) and dimethylformamide (10 ml).High-purity nitrogen was replaced three times, after reacting at 50oC for 16 hours,Extracting the mixture with dichloromethane and water, combining the organic phases, enriching the organic solvent, and further purifying the product by column chromatography. 2-Deutero-3-(ethyl butyrate)-6-chlorotoluene was obtained in a yield of 78%.

The synthetic route of 2-Chloro-6-iodotoluene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anhui Xiulang New Materials Technology Co., Ltd.; Zhang Honghai; Guo Lei; Shui Xinfeng; (15 pag.)CN110054541; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 404337-42-4, A common heterocyclic compound, 404337-42-4, name is 5-Chloro-2-iodo-m-xylene, molecular formula is C8H8ClI, 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 250 mL vessel equipped with a mechanical stirrer, thermometer, distillation head anddropping funnel, solid sodium hydroxide (3.9 g, 0.10 mol, microprills with 0.5- 1 mm diameter) is chargedunder an inert atmosphere.1-Methyl-2-pyrrolidone (NMP, 68 g) is added to the vessel in one portion through the dropping funnel and the reaction mixture cooled to 10 – 15 C while stirring. A solution of malononitrile (NEC-CH2- CEN) (2.27 g, 0.034 mol) in NMP (2.7 g) is added through the dropping funnel over 5 minutes maintainingthe temperature at 10 – 15 C. The reaction mixture is then heated to 100 C and a vacuum (30 mbar) applied, upon which solvent (32 g) is distilled off. The mixture is then heated to 130 C and a stream of nitrogen is passed through.2-lodo-5-chloro-1 ,3-dimethyl-benzene (9.0 g, 95% purity, 0.032 mol) is then added through the dropping funnel over 5 minutes at 130 CC. A mixture containing palladium (II) chloride (0.150 g, solutionin conc. hydrochloric acid, assay 20% Pd, 0.281 mmol), triphenylphosphine (0.186 g, 0.709 mmol) and NMP (13.7 g) is then added through the dropping funnel over a 2-minute period. The temperature is allowed to rise to 130 C and the reaction mixture stirred at this temperature for 80 mm. Conversion is monitored by pulling samples and subsequent HPLC analysis. A second portion of a mixture containing palladium (II) chloride (0.103 g, solution in conc. hydrochloric acid, assay 20% Pd, 0.194 mmol),triphenylphosphine (0.132 g, 0.504 mmol) and NMP (9.76 g) is then added through the dropping funnel over a 2-minute period and the reaction mixture stirred at 130 C for 40 mm.When conversion is complete, a vacuum (20 – 40 mbar) is applied and solvent (38 g) is distilled off. The resulting residue is cooled to 80 C and water (30 g) is added. After cooling to room temperature, the resulting mixture is filtered through a filter paper and the filter cake washed with water (10 g). To thecombined filtrates, hydrochloric acid (9.6 g, assay 32%, 0.084 mol) is added to adjust the pH from 13.3 to 1.3.The resulting mixture is extracted with toluene (50 g). The organic phase is washed with water (2 x 20g) and evaporated to dryness. The resulting solid residue is recrystallized from 1-pentanol (17 g) and the resulting crystals filtered, washed with 1-pentanol (4 g) and dried under vacuum to yield 2-(4-chloro-2,6-dimethyl-phenyl)propanedinitrile (melting point (m.p.) 145 – 147 C).

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:
Patent; SYNGENTA PARTICIPATIONS AG; ZELLER, Martin; FEDOU, Nicolas; (19 pag.)WO2018/15489; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 459424-72-7, name is 1,2,3-Trifluoro-4-iodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 459424-72-7

To a solution of 1, 2, 3-trifluoro-4-iodobenzene (3.3 g, 18.8 mmoL) in 1, 4-dioxane (100 mL) was added 4, 4, 5, 5-tetramethyl-2- (1, 4-dioxaspiro [4.5] dec-7-en-8-yl) -1, 3, 2-dioxaborolane (5 g, 18.8 mmol) , Pd (dppf) Cl2(1.3 g, 1.88 mmol) and Cs2CO3(9.2 g, 28.2 mmol) and the mixture was heated at 70 for 5 hours. Then evaporated the solvent under reduced pressure and the residue was purified by column chromatography (PE: EA=5: 1) to give product as an oil (4.5 g in 88.6%yield) .

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:
Patent; BEIGENE, LTD.; WANG, Hexiang; GUO, Yunhang; REN, Bo; WANG, Zhiwei; ZHANG, Guoliang; ZHOU, Changyou; (353 pag.)WO2018/54365; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 773136-66-6, These common heterocyclic compound, 773136-66-6, name is Ethyl 2-Fluoro-5-iodobenzoate, 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.

10586] Under nitrogen atmosphere, starting Ester Intermediate Se (5.0 g, 15.3 mmol) was dissolved inTHF (40 mE), the reaction mixture was cooled to -50 C. and stirred for 10 minutes. Isopropyl-magnesium-chioride (11 mE of a 2M solution in THF) was added dropwise and the reaction mixture was stirred at -50 C. for 2 h. The reaction mixture was cooled to -78 C. and a solution of cyclobutanone (2.15 g, 30.6 mmol) in THF (10 mE) was added dropwise. The reaction mixture was stirred at -78 C. for 1 h, then warmed to room temperature and stirred for 18 h. The solvent was removed under vacuum, dichloromethane was added and the reaction mixture was washed with a saturated solution of NaHCO3, The organic phase was concentrated under vacuum and the crude product obtained was purified by flash chromatography (eluent from 90:10 to 80:20 Cy/EtOAc) to obtainthe desired product (3.0 g).10587] GC-MS (Method 10): R=10.91 mm10588] MS: mlz=210 (M-28)

The synthetic route of 773136-66-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; GIOVANNINI, Riccardo; BERTANI, Barbara; FRATTINI, Sara; DI ANTONIO, Giustino; US2014/45856; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 59382-39-7, name is 1-Fluoro-4-iodo-2-(trifluoromethyl)benzene, 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 59382-39-7, Computed Properties of C7H3F4I

(69-1) Synthesis of 3-(4-fluoro-3-trifluoromethylphenyl)-2-propyne-1-ol (compound 69-1) A mixture of 2-fluoro-5-iodobenzotrifluoride (5.00 g), copper(I) iodide (65.5 mg), triphenylphosphine (226 mg), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (356 mg), propargyl alcohol (1.12 ml), diisopropylethylamine (12.0 ml) and tetrahydrofuran (80 ml) was stirred at room temperature for 11 hr. The reaction mixture was added to brine, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1 – 80:20) to give the object product (3.26 g) as a brown oil. 1H-NMR(CDCl3) delta (ppm): 1.69(1H, t, J=6.2Hz), 4.50(2H, d, J=6.2Hz), 7.16(1H, t, J=9.3Hz), 7.58-7.62(1H, m), 7.69(1H, dd, J=1.4, 6.8Hz).

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-Fluoro-4-iodo-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; EP2168944; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 1262417-94-6, These common heterocyclic compound, 1262417-94-6, name is Methyl 3-fluoro-6-iodo-2-methylbenzoate, 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 methyl 3-fluoro-6-iodo-2-methylbenzoate i-lOb (0.5 g, 1.7 mmol) in dioxane (5 mL) were added 4,4,4?,4?,5,5,5?,5?-octamethyl-2,2?-bi (1,3,2-dioxaborolane) (0.77g, 3.1 mmol), potassium acetate (217 mg, 2.21 mmol) and PdC12(dppf) (62 mg, 85 umol). The mixture was stirred at 100 C for 18 h under N2. The mixture was filtered and the filtrate was concentrated. The residue was purified by silica gel flash chromatography (1:100-1:20 EtOAc/hexanes) to give the title compound as a solid. ?H NMR (400 MHz, CDC13) oe 7.54-7.62 (m, 1H), 7.06 (t, J= 8.8 Hz, 1H), 3.89 (s, 3H), 2.26 (d, J 1.5 Hz, 3H), 1.32 (s, 12H).

The synthetic route of 1262417-94-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ZHANG, Hongjun; BARR, Kenneth, Jay; LAPOINTE, Blair, T.; GUNAYDIN, Hakan; LIU, Kun; TROTTER, B., Wesley; (67 pag.)WO2017/75185; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 5469-33-0 as follows. Quality Control of (Iodomethyl)cyclohexane

EXAMPLE J-1 Procedure for Preparation of 4(5)-cyclohexylmethyl-1H-imidazole: Procedure- 2-Tert-butyldimethylsilyl-1-dimethylsulfamoyl imidazole (1) (4.1 g, 14.2 mmol) is taken up in 47 mL of anhydrous THF and cooled to -20 C. n-BuLi (8.9 mL, 14.2 mmol) is added dropwise to the solution of (1). The resultant solution is stirred at -20 C. for 45 min. Cyclohexylmethyl iodide (2) (3.14 g, 14 mmol) is then added dropwise to the reaction mixture. Then reaction is warmed to rt and stirred overnight. The next day the reaction is quenched with saturated ammonium chloride and diluted with water. The mixture is extracted with ethyl acetate (3*100 mL). The organic layers are combined and washed with water followed by brine. The organic phase is dried over sodium sulfate and the solvent removed under reduced pressure. Flash chromatography (4:1 ethyl acetate/hexane) affords 2.26 g (5.6 mmol) of 5-cyclohexylmethyl-2-tert-butyldimethylsilyl-1-dimethylsulfamoyl imidazole (3).

According to the analysis of related databases, 5469-33-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Allergan Sales, Inc.; US2002/156076; (2002); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 51738-07-9,Some common heterocyclic compound, 51738-07-9, name is 2-Chloro-6-iodobenzaldehyde, molecular formula is C7H4ClIO, 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.

[0136] To a solution of the appropriate commercially available benzaldehyde or 87 (4.31 mmol) in anhydrous MeOH (15 mL) at rt was added NaOMe (4.31 mmol, 0.5 M in MeOH) and the yellow solution was allowed to stir for 5 min. The appropriate ketone (4.31 mmol) was added dropwise as a solution in MeOH (3 mL). After stirring overnight, the solvent was removed under reduced pressure and the crude was diluted with satd. NH4C1 (20 mL). The aqueous layer was extracted with CH2CI2 (3 x 20 mL) and the combined organic extracts were dried (MgS04) and the solvent distilled off under reduced pressure to afford a crude residue. The crude product was purified by silica flash chromatography to afford the following compounds.

The synthetic route of 51738-07-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NEWLINK GENETICKS CORPORATION; MAUTINO, Mario; KUMAR, Sanjeev; WALDO, Jesse; JAIPURI, Firoz; KESHARWANI, Tanay; WO2012/142237; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 41252-97-5, These common heterocyclic compound, 41252-97-5, name is 4-Iodo-2-nitrotoluene, 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 4-iodo-l-methyl-2-nitro-benzene (25.0 g, 107 mmol) in 300 mL of ethanol was added sulfided platinum (3.00 g) and ammonium formate (20.3 g, EPO 321 mmol). The mixture was heated to reflux for 12 h and then cooled to 22 C, filtered through Celite and concentrated in vacuo. The resulting residue was diluted with H2O (300 mL) and extracted with 3 x 200 mL CH2Cl2. The organic fractions were combined, washed with brine, dried over Na2SO4 and concentrated in vacuo to give b (21.1 g, 95%): MS m/z = 234 (M+H).

The synthetic route of 41252-97-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MILLENNIUM PHARMACEUTICALS, INC.; WO2006/41773; (2006); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 52914-23-5, These common heterocyclic compound, 52914-23-5, name is 2-(4-Iodophenyl)ethanol, 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.

A mixture of 1.14 g (4.60 mmol) of 2-(4-iodophenyl)ethanol, 0.88 g (6.89 mmol) of 4-chlorophenol, 2.99 g (9.20 mmol) of cesium carbonate, 0.14 g (1.38 mmol) of N,N-dimethylglycine and 0.087 g (0.46 mmol) of cuprous iodide in 4 ml of dioxane is heated at 90 C. for 24 hours with thorough stirring under an argon atmosphere. It is cooled to ambient temperature and taken up in 150 ml of ethyl acetate and 50 ml of water. After the phases have settled and been separated, the organic phase is washed with 25 ml of water and 25 ml of saturated aqueous sodium chloride solution, dried over magnesium sulphate and evaporated to dryness. The residue is purified by chromatography on silica gel, eluting with an 85/15 then 75/25 mixture of cyclohexane and ethyl acetate, to give 0.68 g of product in the form of an oil.

The synthetic route of 52914-23-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sanofi-Aventis; US2006/14830; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com