Category: 626-62-0

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. 626-62-0, name is Iodocyclohexane, A new synthetic method of this compound is introduced below., Computed Properties of C6H11I

A mixture of zinc dust (16.34 g, 250 mmol, Aldrich, -325 mesh) and dry tetrahydrofuran (6 mL) under argon was treated with 1,2-dibromoethane (0.94 g, 5 mmol). The zinc suspension was then heated with a heat gun to ebullition, allowed to cool, and heated again. This process was repeated three times to make sure the zinc dust was activated. The activated zinc dust suspension was then treated with trimethylsilyl chloride (0.54 g, 5 mmol), and the suspension was stirred for 15 min at 25 C. The reaction mixture was then treated dropwise with a solution of cyclohexyl iodide (21 g, 100 mmol) in dry tetrahydrofuran (30 mL) over 15 min. During the addition, the temperature rose to 60 C. The reaction mixture was then stirred for 3 h at 40-45 C. The reaction mixture was then cooled to 25 C. and diluted with dry tetrahydrofuran (60 mL). The stirring was stopped to allow the excess zinc dust to settle down (3 h). In a separate reaction flask, a mixture of lithium chloride (8.48 g, 200 mmol, predried at 130 C. under high vacuum for 3 h) and copper cyanide (8.95 g, 100 mmol) in dry tetrahydrofuran (110 mL) was stirred for 10 min at 25 C. to obtain a clear solution. The reaction mixture was cooled to -70 C. and then slowly treated with the freshly prepared zinc solution using a syringe. After the addition, the reaction mixture was allowed to warm to 0 C. where it was stirred for 5 min. The reaction mixture was again cooled back to -70 C. and then slowly treated with methyl propiolate (7.56 g, 90 mmol). The resulting reaction mixture was stirred for 15 h at -70 C. to -50 C. and then slowly treated with a solution of iodine (34.26 g, 135 mmol) in dry tetrahydrofuran (30 mL), with the temperature kept at -70 C. to -60 C. After addition of the iodine solution, the cooling bath was removed, and the reaction mixture was allowed to warm to 25 C. where it was stirred for 2 h. The reaction mixture was then poured into a solution consisting of a saturated aqueous ammonium chloride solution (400 mL) and ammonium hydroxide (100 mL), and the organic compound was extracted into ethyl acetate (3250 mL). The combined organic extracts were successively washed with a saturated aqueous sodium thiosulfate solution (1500 mL) and a saturated aqueous sodium chloride solution (1500 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230-400 mesh, 9/1 hexanes/diethyl ether) afforded (E)-3-cyclohexyl-2-iodo-acrylic acid methyl ester (26.3 g, 99%) as a light pink oil: EI-IIRMS m/e calcd for C10H15IO2 (M+) 294.0117, found 294.0114.

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; Hoffmann-La Roche Inc.; US6353111; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

626-62-0, name is Iodocyclohexane, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C6H11I

The compound 4b (0.180 g, 0.52 mmol), iodocyclohexane (0.110 g, 0.52 mmol) and potassium carbonate (0.072 g, 0.52 mmol) were added to dimethylformamide (2 mL). The mixture was refluxed under stirring for 12 h at 80 C, acidified with concentrated hydrochloric acid to pH 3-4; the resulting solid was filtered, collected, washed with water, dried, and crystallized from petroleum ether to give 10 as white crystals.

The synthetic route of 626-62-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Barone, Mariarita; Pistara, Venerando; Frasca, Giuseppina; Noto, Clio; Scribano, Maria; Catalfo, Alfio; Santagati, Andrea; Medicinal Chemistry Research; vol. 24; 6; (2015); p. 2461 – 2475;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-62-0, A common heterocyclic compound, 626-62-0, name is Iodocyclohexane, molecular formula is C6H11I, 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 the glove box, t-BuOLi (1 mmol, 2 equivalents, 80.1 mg) was added to the vial containing the stirrer in turn.B2pin2 (2mmol, 4 equivalents, 507.9mg), 0.85mL solvent methanol, 10muL H2O,Iodocyclohexane (0.5 mmol).The capped vial was removed from the glove box and the reaction mixture was stirred at 50 C for 48 hours. After cooling to room temperature, the reaction mixture was transferred to a test tube by methanol, and a certain amount of internal standard n-decane was added and diluted with ethyl acetate.The yield of the product cyclohexylboronic acid pinacol ester was determined by a GC-fid method to be 30%.

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; Peking University; Mo Fanyang; Sun Beiqi; Liu Qianyi; Hong Junting; (10 pag.)CN109575063; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 626-62-0, name is Iodocyclohexane, 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. Safety of Iodocyclohexane

General procedure: A 2 mL crimp-top GC vial was charged with NiBr2(DME) (6.2 mg, 0.02 mmol, 0.1 equiv), dppf (11 mg, 0.02 mmol, 0.1 equiv), and activated Zn powder [35] (26.2 mg, 0.4 mmol, 2 equiv). The vial was crimped shut and the olefin (0.2 mmol, 1 equiv) was injected through the septum as a solution in 0.3 mL THF followed by 0.2 mL HFIP. The iodide (1-2 equiv) was then added (as a solution in THF, if solid) and the vial was shaken at 1000 rpm for 12 h at 25 C. The reaction was diluted with EtOAc and quenched by the addition of 1 M HCl (aq). The aqueous phase was extracted with three portionsof EtOAc. The combined organic phase was then passed through a plug of silica. An aliquot of the organic phase was used for GC or GC/MS analysis with mesitylene as an internal standard. Solvent was removed and the mixture was purified by chromatography on silicagel with EtOAc/hexane as the eluent to give the products as colorless oils.

The synthetic route of Iodocyclohexane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Diccianni, Justin B.; Chin, Mason; Diao, Tianning; Tetrahedron; vol. 75; 31; (2019); p. 4180 – 4185;,
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. 626-62-0, name is Iodocyclohexane, A new synthetic method of this compound is introduced below., COA of Formula: C6H11I

A mixture of zinc dust (16.34 g, 250 mmol, Aldrich, -325 mesh) and dry tetrahydrofuran (6 mL) under argon was treated with 1,2-dibromoethane (0.94 g, 5 mmol). The zinc suspension was then heated with a heat gun to ebullition, allowed to cool, and heated again. This process was repeated three times to make sure the zinc dust was activated. The activated zinc dust suspension was then treated with trimethylsilyl chloride (0.54 g, 5 mmol), and the suspension was stirred for 15 min at 25 C. The reaction mixture was then treated dropwise with a solution of cyclohexyl iodide (21 g, 100 mmol) in dry tetrahydrofuran (30 mL) over 15 min. During the addition, the temperature rose to 60 C. The reaction mixture was then stirred for 3 h at 40-45 C. The reaction mixture was then cooled to 25 C. and diluted with dry tetrahydrofuran (60 mL). The stirring was stopped to allow the excess zinc dust to settle down (3 h). In a separate reaction flask, a mixture of lithium chloride (8.48 g, 200 mmol, predried at 130 C. under high vacuum for 3 h) and copper cyanide (8.95 g, 100 mmol) in dry tetrahydrofuran (110 mL) was stirred for 10 min at 25 C. to obtain a clear solution. The reaction mixture was cooled to -70 C. and then slowly treated with the freshly prepared zinc solution using a syringe. After the addition, the reaction mixture was allowed to warm to 0 C. where it was stirred for 5 min. The reaction mixture was again cooled back to -70 C. and then slowly treated with methyl propiolate (7.56 g, 90 mmol). The resulting reaction mixture was stirred for 15 h at -70 C. to -50 C. and then slowly treated with a solution of iodine (34.26 g, 135 mmol) in dry tetrahydrofuran (30 mL), with the temperature kept at -70 C. to -60 C. After addition of the iodine solution, the cooling bath was removed, and the reaction mixture was allowed to warm to 25 C. where it was stirred for 2 h. The reaction mixture was then poured into a solution consisting of a saturated aqueous ammonium chloride solution (400 mL) and ammonium hydroxide (100 mL), and the organic compound was extracted into ethyl acetate (3250 mL). The combined organic extracts were successively washed with a saturated aqueous sodium thiosulfate solution (1500 mL) and a saturated aqueous sodium chloride solution (1500 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230-400 mesh, 9/1 hexanes/diethyl ether) afforded (E)-3-cyclohexyl-2-iodo-acrylic acid methyl ester (26.3 g, 99%) as a light pink oil: EI-IIRMS m/e calcd for C10H15IO2 (M+) 294.0117, found 294.0114.

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; Hoffmann-La Roche Inc.; US6353111; (2002); B1;,
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. 626-62-0, name is Iodocyclohexane, A new synthetic method of this compound is introduced below., Product Details of 626-62-0

General procedure: A mixture of alkyl/aryl halide, 1 (1.2 mmol), ammonium hydroxide (1 mmol) and nanosulfur powder (3 mmol, 96 mg) was stirred in 5mL of solvent (ethanol/water (2:1)) at 60 C. Under this stirring condition indium oxide nanoparticles (3 mol-%) were added to it and the reaction was stirred for a period of 10 min to 1 h at 60 C. After completion of the reaction as indicated by thin layer chromatography (TLC), the reaction mixture was cooled to room temperature and a 2:1 mixture of ethyl acetate/water (15 mL) was added and indium oxide was removed by centrifuge. The combined organic extracts were dried with anhydrous sodium sulfate and concentrated to give desired product in high purity.

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 626-62-0, 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. 626-62-0, name is Iodocyclohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 2 mL crimp-top GC vial was charged with NiBr2(DME) (6.2 mg, 0.02 mmol, 0.1 equiv), dppf (11 mg, 0.02 mmol, 0.1 equiv), and activated Zn powder [35] (26.2 mg, 0.4 mmol, 2 equiv). The vial was crimped shut and the olefin (0.2 mmol, 1 equiv) was injected through the septum as a solution in 0.3 mL THF followed by 0.2 mL HFIP. The iodide (1-2 equiv) was then added (as a solution in THF, if solid) and the vial was shaken at 1000 rpm for 12 h at 25 C. The reaction was diluted with EtOAc and quenched by the addition of 1 M HCl (aq). The aqueous phase was extracted with three portionsof EtOAc. The combined organic phase was then passed through a plug of silica. An aliquot of the organic phase was used for GC or GC/MS analysis with mesitylene as an internal standard. Solvent was removed and the mixture was purified by chromatography on silicagel with EtOAc/hexane as the eluent to give the products as colorless oils.

The synthetic route of Iodocyclohexane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Diccianni, Justin B.; Chin, Mason; Diao, Tianning; Tetrahedron; vol. 75; 31; (2019); p. 4180 – 4185;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 626-62-0, A common heterocyclic compound, 626-62-0, name is Iodocyclohexane, molecular formula is C6H11I, 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.

General procedure: In a dry 10 mL round bottomflask, 1 (0.2 mmol), Na2S2O3 (0.21 mmol),CF3SiMe3 (0.4 mmol), CuCl/Phen(5% mol) and K3PO4 (0.3 mmol) were added sequentially andthen dissolved in 2 mL DMSO. The resulting mixture was stirred at 80 oCunder air and monitored by TLC. Purification by column chromatography on silicagave rise to 2.

The synthetic route of 626-62-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhong, Wei; Liu, Xiaoming; Tetrahedron Letters; vol. 55; 35; (2014); p. 4909 – 4911;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 626-62-0, name is Iodocyclohexane, 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 626-62-0, Application In Synthesis of Iodocyclohexane

In a round bottomed 500 ml flask equipped with stir bar and containing 100 ml acetone, was added 7.6 g of ammonium thiocyanate salt and stirred at room temperature until the complete dissolution of salt. To this clear solution, 10 g of montmorillonite K10 clay was added in portions over 10 min with stirring. After complete addition, the formation of reddish suspension was observed which was vigorously stirred for another 30 min at room temperature. Then the suspension is placed in a rotary vacuum evaporator and the solvent was removed under reduced pressure. The dry solid crust adhering to the walls of the flask was flaked off with a spatula, and solvent evaporation was resumed. After complete drying, yielded, about 17.6 g of clay supported ammonium thiocyanate as a light red free flowing powder which shows no loss of reactivity after standing in an open powder box for one week.; Phenacyl bromide (1 mmol) and K10-montmorillonite clay supported ammonium thiocyanate (3 mmol) were taken in mortar, mixed with spatula, and ground with pestle for stipulated time (see Table 3). After complete conversion as indicated by TLC, the solid reaction mixture was directly loaded on silica gel column by avoiding aqueous work up-extraction step. Later elution with ethyl acetate-hexane (9:1-3:1) solvent system and evaporation of solvents in rotary vacuum evaporator afforded pure phenacyl thiocyanate (99%). Same procedure as discussed above was followed to prepare all thiocyanate compounds shown in this work. All compounds prepared were characterized by IR, Mass, and NMR spectroscopy.

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, Iodocyclohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Meshram; Thakur, Pramod B.; Madhu Babu; Bangade, Vikas M.; Tetrahedron Letters; vol. 53; 14; (2012); p. 1780 – 1785;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-62-0, These common heterocyclic compound, 626-62-0, name is Iodocyclohexane, 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.

General procedure: THF (1.5 mL), organic halide 3 (1.5 mmol, 1.0 equiv) and Ir(dtbbpy)(ppy)2 PF6 (3.5 mg, 0.0025 equiv) were successively added to a test tube containing Zn dust (73 mg, 1.125 mmol, 0.75 equiv). The reaction mixture was stirred under irradiation with a strip of 400 nm LEDs for 5 h, with water cooling to maintain the reaction temperature around 23-25 C. For the work-up, H2O (5 mL) was added and the mixture was extracted with hexane (3 ¡Á 7 mL). The combined extracts were filtered through Na2SO4 and concentrated under vacuum.The residue was purified by flash chromatography eluting with hexane/EtOAc.

The synthetic route of 626-62-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Levin, Vitalij V.; Agababyan, Daniil P.; Struchkova, Marina I.; Dilman, Alexander D.; Synthesis; vol. 50; 15; (2018); p. 2930 – 2935;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com