Category: 627-31-6

Synthetic Route of 627-31-6, 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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), This compound has unique chemical properties. The synthetic route is as follows.

Example 7; [0055] Synthesis of 3-(benzyloxy)-1 -(3-iodopropyl)pyridin-2(1 H)-one(Compound 7); To a solution of 1 ,3-diiodopropane (7.1 ml_, 63 mmol) in tetrahydrofuran (50 ml_) was added 3-(benzyloxy)pyhdin-2(1 H)-one (1.28 g, 6.3 mmol) and Na2CO3 (0.67 g, 6.3 mmol). The mixture was then stirred at 70 0C for 1 day. Reaction progress was monitored by ES-MS. After ESMS showed essentially complete consumption of the starting material 3-(benzyloxy)pyhdin-2(1 H)-one, the reaction was stopped. Then the reaction mixture was filtered, concentrated, and subjected to flash column chromatography (eluent: hexane : ethylacetate 1 :1 ). Compound 7 was obtained (240 mg, 10% yield). Analysis: ES-MS (positive ion in MeOH/H2O): m/z = 370.2, ([M+H]+, calculated: 370.03).

The chemical industry reduces the impact on the environment during synthesis 1,3-Diiodopropane(stabilized with Copper chip). I believe this compound will play a more active role in future production and life.

Reference:
Patent; BOARD OF SUPERVISORS OF LOUISIANA STATE UNIVERSITY AND ARGRICULTURAL AND MECHANICAL COLLEGE; WO2008/100907; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 627-31-6, These common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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.

Diiodopropane (0.52 mL, 4.50 mmol, 5 eq) and potassium carbonate (124 mg, 0.90 mmol, 1 eq) were added to a solution of phenol 40 (500 mg, 0.90 mmol) in acetone (5 mL, dried over molecular sieves). The reaction mixture was then warmed to 60C and stirred for 3 hours. Acetone was removed by rotary evaporation under reduced pressure. The resulting residue was subjected to flash column chromatography (silica gel; 50/50, v/v, hexane/ethyl acetate,). Pure fractions were collected and combined and excess eluent was removed to provide 42 (450 mg, 70% with some impurities due to elimination reaction). LC/MS, method 2, 3.90 min (ES+) m/z (relative intensity) 722.33 ([M+H]+, 100).

Statistics shows that 1,3-Diiodopropane(stabilized with Copper chip) is playing an increasingly important role. we look forward to future research findings about 627-31-6.

Reference:
Patent; SPIROGEN SARL; HOWARD, Philip Wilson; TIBERGHIEN, Arnaud; WO2013/53872; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 627-31-6, 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.

Methyl 2-(4-bromo-2-nitrophenyl)acetate (2 g, 7.3 mmol, Eq: 1) and 1,3-diiodopropane (2.45 g, 956 mu, 8.03 mmol, Eq: 1.10) were combined with dimethylformamide (20 ml) at 0 C. Sodium hydride (1.17 g, 29.2 mmol, Eq: 4.00) was slowly added. The dark blue reaction mixture was heated to room temperature and stirred for 16h. The reaction mixture was poured into water and extracted with ethyl acetate (3x). The organic layers were combined and washed with brine, dried over sodium sulfate, filtered and concentrated in vacuo. (0328) The residue was purified by chromatography on silica gel to afford the desired product as a brown solid (285 mg, 12 %).

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.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; GAUFRETEAU, Delphine; HILPERT, Hans; HUMM, Roland; KOLCZEWSKI, Sabine; MUSER, Thorsten; PLANCHER, Jean-Marc; STOLL, Theodor; (63 pag.)WO2017/76932; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 627-31-6, The chemical industry reduces the impact on the environment during synthesis 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), I believe this compound will play a more active role in future production and life.

General procedure: The mixture of 4-methylpiperazine-1-carbodithioate (2.21 gm, 11.16 mmol) and diiodomethane (0.3 mL, 3.72 mmol) in CH3CN (20 mL) was stirred at room temperature for overnight. The reaction mixture was concentrated under reduced pressure, crude product was treated with water (10 mL) and extracted with EtOAc (10 * 3 mL). EtOAc layer was washed with water (5 * 3 mL) and combined organic layers were dried on anhydrous sodium sulfate, filtered, and concentrated. The crude product was purified over column chromatography (100-200 mesh) using MeOH/CHCl3 as eluent to afford compound as white solid (0.76 g, 56%); 4.1.53 Propane-1,3-diyl bis(4-(3-cyanopropyl)piperazine-1-carbodithioate) (56) The title compound was synthesized from sodium 4-(3-cyanopropyl)piperazine-1-carbodithioate and diiodopropane in 56% yield as white solid; mp: 118-120 C; IR (KBr) nu (cm-1): 2942, 2823, 2248, 1646; 1H NMR (300 MHz, CDCl3 + CCl4): delta 4.34-4.05 (8H, m), 3.40 (4H, t, J = 7.1 Hz), 2.55-2.42 (16H, m), 2.16-2.07 (2H, m), 1.88-1.79 (4H, m); 13C NMR (75 MHz, CDCl3 + CCl4): delta 196.5 (C=S), 119.1, 55.9, 52.6, 50.7, 35.9, 28.2, 22.7, 15.0; ESI-MS: (m/z)499 (MH+); Anal. (%) calcd. for C21H34N6S4: C, 50.57; H, 6.87; N, 16.85; found C, 50.68; H, 6.94; N, 16.75.

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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Article; Lal, Nand; Jangir, Santosh; Bala, Veenu; Mandalapu, Dhanaraju; Sarswat, Amit; Kumar, Lalit; Jain, Ashish; Kumar, Lokesh; Kushwaha, Bhavana; Pandey, Atindra K.; Krishna, Shagun; Rawat, Tara; Shukla, Praveen K.; Maikhuri, Jagdamba P.; Siddiqi, Mohammad I.; Gupta, Gopal; Sharma, Vishnu L.; European Journal of Medicinal Chemistry; vol. 115; (2016); p. 275 – 290;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 627-31-6, 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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip) belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

methyl 2-(4-bromo-2-nitrophenyl)acetate (2 g, 7.3 mmol, Eq: 1) and 1,3-diiodopropane (2.45 g, 956 muL, 8.03 mmol, Eq: 1.10) were combined with dimethylformamide (20 mL) at 0C. Sodium hydride (1.17 g, 29.2 mmol, Eq: 4.00) was slowly added. The dark blue reaction mixture was heated to room temperature and stirred for 16h. The reaction mixture was poured into water and extracted with ethyl acetate (3x). The organic layers were combined and washed with brine, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel to afford the desired product as a brown solid (285 mg, 12%).

The synthetic route of 1,3-Diiodopropane(stabilized with Copper chip) has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; GAUFRETEAU, Delphine; HILPERT, Hans; HUMM, Roland; KOLCZEWSKI, Sabine; MUSER, Thorsten; PLANCHER, Jean-Marc; STOLL, Theodor; (55 pag.)WO2017/76931; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 627-31-6, 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. 627-31-6 name is 1,3-Diiodopropane(stabilized with Copper chip), 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.

The synthesis method of the ionic liquid-based Gemini cationic surfactant of this embodiment is as follows:(1) 59.18 g (0.2 mol) of 1,3-diiodopropane and 20 g of ethanol were added to a four-neck round bottom flask.The mixture was heated to boiling with stirring, and 1 g of tetrabutylammonium iodide was added.Add 24.1g (0.1mol) dropwiseN,N-dimethyltetradecyl tertiary amine,The reflux temperature was maintained, and after stirring for 8 hours, ethanol was distilled off under reduced pressure.The solid was washed three times with chloroform.The filter cake was dried under vacuum at 60 C for 6 hours to obtain an intermediate N,N-dimethyl(1-iodopropyl)tetradecyl ammonium iodide in a yield of 96.5%;

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

Reference:
Patent; Zhengzhou University of Light Industry; Yang Xuzhao; Wang Jun; Li Yakun; Ping Dan; Zhang Yingying; Wu Shide; (8 pag.)CN109970657; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 627-31-6, The chemical industry reduces the impact on the environment during synthesis 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), I believe this compound will play a more active role in future production and life.

Diiodopropane (0.295 g, 1.00 mmol, 5.0 eq) and potassium carbonate (0.028 g, 0.20 mmol, 1.0 eq) were added to a solution of the phenol 12 (0.100 g, 0.020 mmol, 1 .0 eq) in dry acetone (5 mL). The reaction mixture was heated at 60C for 6 hours when LC/MS showed complete reaction. The reaction mixture was concentrated to dryness under reduced pressure and the residue was purified by flash chromtography (silica gel, 75/25 v/v n- hexane/EtOAc to 50/50 v/v n-hexane/EtOAc) to afford the product as a colourless oil (0.074 g, 56%). LC/MS (3.853 min (ES+)), m/z: 669.0 [M+H]+. 1H NMR (400 MHz, CDCI3) delta 7.26 (s, 1 H), 6.90 (s, 1 H), 6.68 (s, 1 H), 6.24 (d, 1 H, J = 15.3 Hz), 5.87 (d, 1 H, J = 8.9 Hz), 5.78 (m, 1 H), 5.53 (m, 1 H), 5.12 (m, 2H), 4.65 (m, 2H), 4.41 (m, 1 H), 4.1 1 (m, 1 H), 3.93 (s, 3H), 3.81 (m, 1 H), 3.40 (t, 2H, J = 6.7 Hz), 3.05 (dd, 1 H, J = 16.3, 10.1 Hz), 2.57 (m, 1 H), 2.34 (m, 2H), 1 .84 (d, 3H, J = 6.6 Hz), 0.92 (s, 9H), 0.28 (s, 3H), 0.26 (s, 3H).

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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SPIROGEN SARL; HOWARD, Philip Wilson; TIBERGHIEN, Arnaud; WO2013/53872; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 627-31-6, 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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip) belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Diiodopropane (0.295 g, 1.00 mmol, 5.0 eq) and potassium carbonate (0.028 g,0.20 mmol, 1.0 eq) were added to a solution of the phenol 33 (0.100 g, 0.020 mmol, 1.0 eq) in dry acetone (5 mL). The reaction mixture was heated at 60C for 6 hours when LC/MS showed complete reaction. The reaction mixture was concentrated to dryness under reduced pressure and the residue was purified by flash chromatography (silica gel,75/25 v/v n-hexane/EtOAc to 50/50 v/v n-hexane/EtOAc) to afford the product as acolourless oil (0.074 g, 56%). LC/MS (3.853 mm (ESj), m/z: 669.0 [M+H]. ?H NMR(400 MHz, CDC13) oe 7.26 (s, 1H), 6.90 (s, 1H), 6.68 (s, 1H), 6.24 (d, 1H, J = 15.3 Hz),5.87 (d, 1H, J= 8.9 Hz), 5.78 (m, 1H), 5.53 (m, 1H), 5.12 (m, 2H), 4.65 (m, 2H), 4.41 (m,1H), 4.11 (m, 1H), 3.93 (s, 3H), 3.81 (m, 1H), 3.40 (t, 2H, J 6.7 Hz), 3.05 (dd, 1H, J16.3, 10.1 Hz), 2.57 (m, 1H), 2.34 (m, 2H), 1.84 (d, 3H, J= 6.6 Hz), 0.92 (s, 9H), 0.28 (s,3H), 0.26 (s, 3H).

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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Patent; STEM CENTRX, INC.; SPIROGEN SARL; TORGOV, Michael; HOWARD, Philip Wilson; WO2014/130879; (2014); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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 627-31-6, Application In Synthesis of 1,3-Diiodopropane(stabilized with Copper chip)

Methyl 2-(4-nitrophenyl)acetate (6.0 g, 31 mmol) was dissolved in DMF (100 mL). The solution was cooled to 0 C in an ice bath. NaH (2.50 g, 62.5 mmol, 60% in mineral oil) was added slowly and cautiously. The resulting mixture was allowed to warm to RT and stirred for 15 min. The mixture was cooled again to 0 C and 1,3-diiodopropane (6.0 mL, 52 mmol) was added dropwise. The resulting mixture was allowed to stir at 0 C for 30 min, then 0 C to 10 C for 1.5 h. The solution was cooled to 0 C and quenched with water. The reaction mixture was extracted with DCM (30 mL x3). The combined organic layers were washed with water, brine, dried over Na2SC>4, filtered and concentrated in vacuo to afford a residue. The residue was purified by column chromatography on silica gel (EtOAc in hexane, 0-20% gradient) to afford methyl l-(4-nitrophenyl)cyclobutanecarboxylate.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ZHOU, Hua; ACHAB, Abdelghani; FRADERA, Xavier; HAN, Yongxin; LI, Derun; MCGOWAN, Meredeth, A.; SCIAMMETTA, Nunzio; SLOMAN, David, L.; YU, Wensheng; (98 pag.)WO2019/27855; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C3H6I2

To a mixture of 1,3-diiodopropane (4.4 mL, 38.4 mmol) andethyl 2-oxocyclopentanecarboxylate (0.95 mL, 6.4 mmol) in acetone(16 mL) was added K2CO3 (2.3 g, 16.7 mmol), and the reactionmixture was heated under reflux for 3 days. The mixture was filtered,and the filtrate was then concentrated. The residue was purifiedby silica gel chromatography eluting with 0-50% EtOAc/hexanes to give 28 (1.44 g, 62%). 1H NMR (500 MHz, CDCl3) d4.25-4.10 (m, 2H), 3.16 (qt, J = 9.6, 6.8 Hz, 2H), 2.56-2.40 (m,2H), 2.34-2.24 (m, 1H), 2.08-1.86 (m, 5H), 1.82-1.72 (m, 1H),1.71-1.64 (m, 1H), 1.71-1.64 (m, 1H), 1.26 (t, J = 7.1 Hz, 3H).LC/MS m/z: (M+H)+ calcd for C11H18IO3, 325.03; found 325.0.

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 627-31-6.

Reference:
Article; Wu, Yong-Jin; Guernon, Jason; McClure, Andrea; Luo, Guanglin; Rajamani, Ramkumar; Ng, Alicia; Easton, Amy; Newton, Amy; Bourin, Clotilde; Parker, Dawn; Mosure, Kathleen; Barnaby, Omar; Soars, Matthew G.; Knox, Ronald J.; Matchett, Michele; Pieschl, Rick; Herrington, James; Chen, Ping; Sivarao; Bristow, Linda J.; Meanwell, Nicholas A.; Bronson, Joanne; Olson, Richard; Thompson, Lorin A.; Dzierba, Carolyn; Bioorganic and Medicinal Chemistry; vol. 25; 20; (2017); p. 5490 – 5505;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com