Category: 628-77-3

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 628-77-3 as follows. Application In Synthesis of 1,5-Diiodopentane

Potassium carbonate (2.5 eq) was added to a solution of 8 (1.0 g, 1.72 mmol, 2.1 eq) and either 1,3-dibromopropane; 1,5-diiodopentane; or 1,3-bis(bromomethyl)benzene (1.0 eq) in DMF (5 mL). The resulting mixture was stirred at 75C for 3 days. After diluting with dichloromethane (25 mL), the inorganics were removed by filtration and the filtrate evaporated to dryness under reduced pressure. The residue was purified by flash chromatography to leave the products as white solids. i) diallyl 8,8′-(propane-1,3-diylbis(oxy))(2S,2’S, 11S, 11aS, 11’S, 11 a’S)-bis(2-(benzoyloxy)- 11-((tert-butyldimethylsilyl)oxy)-7-methoxy-5-oxo-2,3, 11, 11 a-tetrahydro-1H- benzo[e]pyrrolo[1,2-a][1,4]diazepine-10(5H)-carboxylate) 9a (gradient: ethyl acetate / heptane, 50/50 to 100/0 v/v). Yield 0.88 g (90%). LC/MS rt 2.17 min m/z (1227.4) M+Na.

According to the analysis of related databases, 628-77-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MEDIMMUNE LIMITED; HOWARD, Philip Wilson; HUTCHINSON, Ian; (102 pag.)WO2020/79239; (2020); 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. 628-77-3, name is 1,5-Diiodopentane, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,5-Diiodopentane

Potassium carbonate (5.03 g, 36.44 mmol, 1.1 eq.) was added to a stirred solution of phenol (2) (14 g, 33.13 mmol, 1.0 eq.) and 1 ,5 diiodopentane (21.46 g, 9.86 mL, 66.26 mmol, 2.0 eq.) in DMF (250 mL). The solution was heated at 70C for 3.5h. The solution was poured into a mixture of ice/water (800 mL) and extracted with EtOAc (4 x 500 mL). The combined extracts were washed with H2O (2 x 250 mL), saturated brine (400 mL), dried (MgS04) and evaporated under reduced pressure to give a brown oil. Purification by flash column chromatography [n-heptane/EtOAc 40% to 80% in 10% increments] gave the product as a yellow foam (12.7 g, 85%). Analytical Data: LC/MS, RT 2.16 min; MS (ES+) m/z (relative intensity) 913 {[M + H]+, 100); 935 {[M + Na])+, 100).

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 628-77-3.

Reference:
Patent; MEDIMMUNE LIMITED; MASTERSON, Luke; VIJAYAKRISHNAN, Balakumar; CHRISTIE, Ronald, James; (118 pag.)WO2019/224340; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 628-77-3, 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. 628-77-3 name is 1,5-Diiodopentane, 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.

Compound 259a:[332] In a smal] vial dissolved Compound 8 (0.100 g, 0.340 mmol) in DMF (5 ml) with stirring at room temperature. 1,5-diiodopentane (0.506 ml, 3.40 mmol) was added fol]owed by the addition of potassium carbonate (0.070 g, 0.510 mmol). The reaction was covered in foil and stirred at room temperature overnight. The reaction was diluted with dichloromethane and washed with aqueous ammonium chloride and brine. The organic layer was dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by silica ptlc using 50% ethyl acetate in hexane to give Compound 259a (0.045 g, 7.32 mumol, 27 % yield). 1H NMR (400 MHz, CDCl3): delta 1.64 (m, 2H), 1.94 (M, 4H), 3.24 (t, 2H, J = 6.5 MHz), 3.52 (dd, IH, J = 4.0, 16.6 MHz), 3.73 (dd, IH, J = 10.5, 16.6 MHz), 3.98 (s, 3H), 4.12 (m, 2H), 4.50 (dt, IH, J = 4.0, 11.2 MHz), 6.84 (s, IH), 7.13 (t, IH, J = 6.0 MHz), 7.29 (m, 2H), 7.57 (s, IH), 7.90 (d, IH, J = 4.4 MHz), 8.29 (d, IH, J = 8.0 MHz). MS (m/z), found 533.3 ([M]++K).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,5-Diiodopentane, and friends who are interested can also refer to it.

Reference:
Patent; IMMUNOGEN, INC.; LI, Wei; FISHKIN, Nathan, Elliott; ZHAO, Robert, Yongxin; MILLER, Michael, Louis; CHARI, Ravi, V., J.; WO2010/91150; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 628-77-3, A common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, molecular formula is C5H10I2, 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: At room temperature and under nitrogen atmosphere, 12.5 mmol of menthol in 25 mL of THF was added dropwise to a solution containing 24.4 mmol of oil-free KH suspended in 25 mL of THF. When hydrogen evolution had ceased, the reaction mixture was cooled to -50 C and 12.5 mmol of TCE dissolved in 15 mL of THF was slowly added. Once the addition was completed, the cooling bath was removed and the solution was stirred for 1 h at room temperature. The reaction mixture was then cooled to -78 C and a freshly titrated solution of BuLi (30.0 mmol) was added dropwise. After stirring for 30 min at -78 C and 30 min at -50 C, 40.5 mmol of HMPA was added. After stirring for 15 min, the following solution was added: 25 mmol of diiodoalkane (diiodobutane or diiodopentane) in 5.4 mL of THF. The cooling bath was removed and stirred at room temperature for 24 h under nitrogen atmosphere. The solution was then treated with 15 mL of water. The layers were separated. The aqueous phase was extracted thrice with hexanes. The combined organic layers were successively washed with water and brine, and dried over anhydrous MgSO4. Crude product was then purified with flash chromatography using hexanes as eluent.

The synthetic route of 628-77-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hanna, Rana; Daoust, Benoit; Tetrahedron; vol. 67; 1; (2011); p. 92 – 99;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Recommanded Product: 628-77-3

Preparation of Intermediate methyl 1-(4-bromoDhenyl)cvclohexanecarboxylate (1AE-1); Sodium hydride (12 g, 52 mmol) was suspended in tetrahydrofuran (200 mL) under argon and warmed to 35C. Methyl 2-(4-bromophenyl)acetate (26mmol) in tetrahydrofuran added drop wise to reaction over 1 hour. The reaction mixture was then kept at this temperature for 1 hour until all gas evolution has ceased. The 1 ,5- diiodopentane (17 g, 52 mmol) was then added drop wise as a solution in tetrahydrofuran (100 mL) and the reaction mixture stirred at 35C for a further hour and at ambient temperature overnight. After this time, the reaction mixture was cooled to 00C and quenched by the addition of dry silica, filtered and the solvent removed under vacuum. The crude product was then purified by flash chromatography eluting with 33% ethyl acetate in heptane to give methyl 1-(4-bromophenyl)cyclohexanecarboxylate (1AC-1 ) (15.3 g, 99 % yield) as a yellow oil.1 H NMR (400 MHz, CDCI3): 7.45-7.38 (m, 2 H), 7.27-7.24 (m, 2 H), 3.63 (s, 3 H), 2.43 (d, J = 13.3 Hz, 2 H), 1.71-0.80 (m, 8 H) ppm.

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.

Reference:
Patent; PFIZER INC.; ASPNES, Gary, Erik; DOW, Robert, Lee; MUNCHHOF, Michael, John; WO2010/86820; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 628-77-3, 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. 628-77-3, name is 1,5-Diiodopentane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1 ,5-diiodopentane (1 .54 mL, 3.35 g, 10.4 mmol) was added to a stirred solution of the phenol 12 (8.74 g, 20.7 mmol), TBAI (750 mg, 2.05 mmol) and K2003 (3.15 g, 22.8 mmol) in dry DMF (60 mL). The reaction mixture was heated to 70 00 and stirred under an argon atmosphere for 16 hours at which point analysis by LC/MS revealed substantial productformation at retention time 2.21 minutes, ES+ mlz 935 [M+ Na], 913 [M+ H]. The reaction mixture was allowed to cool to room temperature and the DMF was removed by evaporation in vacuo. The resulting residue was red issolved in EtOAc (200 mL) and the aqueous phase was washed with water (3 x 40 mL), brine (50 mL), dried (MgSO4), filtered and evaporated in vacuo to provide the crude product. Purification by lsoleraTM(Hexane/EtOAc, SNAP Ultra 100 g, 100 mL per minute) gave the bis-ether 13 (eluting at60% Hexane/EtOAc) as a yellow foam (6.75 g, 71% yield).

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, 1,5-Diiodopentane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MEDIMMUNE LIMITED; HOWARD, Philip Wilson; GREGSON, Stephen John; (228 pag.)WO2018/69490; (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. 628-77-3, name is 1,5-Diiodopentane, A new synthetic method of this compound is introduced below., Quality Control of 1,5-Diiodopentane

To a solution of 31 (400mg, 1 .5 mmol) in anhydrous DMF (4 mL), in a flask purged with argon, was added K2C03 (320 mg, 1.5 mmol) and 1 ,5-diiodopentane 32 (1.1 mL, 7.6 mmol). The reaction mixture was heated to 60C until complete (30 minutes). The solution was diluted with CH2CI2 (50 mL) and washed with H20 (50 mL) and brine (50 mL) before the organics were dried with MgS04, filtered and the volatiles remove in vacuo. The crude material was purified by silica gel column chromatography (Hexane/EtOAc ; 100% to 3:7) to afford pure product 33 as a light brown foamy gum (61 1 mg, 87% yield). Analytical Data: RT 1 .51 min; MS (ES+) m/z (relative intensity) 458.95 ([M + H]+ , 100 ).

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; SPIROGEN SARL; HOWARD, Philip Wilson; WO2014/96365; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Product Details of 628-77-3

(S) – (4-hydroxy-5-methoxy-2-nitrophenyl) (2- (hydroxymethyl) -4-methylenepyrrolidin-1-yl) methanone (0.801 g, 2.60 mmol) in butanone (10 ml) was added Cs 2CO 3, (2.50 g, 7.67 mmol) , followed by addition of 1, 5-diiodopentane (415 mmol, 1.28 mmol) . The mixture was stirred for 26 h, concentrated and purified on SiO 2 column eluted with MeOH/CH 2Cl 2 (1: 15 to 1: 5) to afford the title compound (0.675 g, 77%yield, 95%pure) . MS ESI m/z calcd for C 33H 41N 4O 12 [M+H] + 685.26, found 685.60.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,5-Diiodopentane, and friends who are interested can also refer to it.

Reference:
Patent; HANGZHOU DAC BIOTECH CO., LTD; ZHAO, Robert Yongxin; ZHUO, Xiaotao; YANG, Qingliang; ZHAO, Linyao; HUANG, Yuanyuan; YE, Hangbo; YANG, Chengyu; LEI, Jun; GAI, Shun; GUO, Huihui; JIA, Junxiang; BAI, Lu; XIE, Hongsheng; ZHOU, Xiaomai; GUO, Zhixiang; LI, Wenjun; CAO, Mingjun; ZHENG, Jun; YE, Zhichang; YANG, Yanlei; (325 pag.)WO2020/6722; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, COA of Formula: C5H10I2

16.1: Methyl (R)-3-tert-butoxycarbonylamino-2-piperidin-1-ylpropanoate 3.1 ml (20.6 mmol) of 1,5-diiodopentane are added to a solution of 5.0 g (19.6 mmol) of commercial methyl (R)-2-amino-3-tert-butoxycarbonylaminopropanoate hydrochloride and 0.22 g (0.6 mmol) of tetrabutylammonium chloride in 50 ml of N,N-diisopropylethylamine. The reaction medium is heated at 127 C. for 5 h and then at 100 C. for 18 h. After evaporation of a maximum amount of N,N diisopropylethylamine, the reaction medium is hydrolyzed and then diluted with ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate, filtered and concentrated under vacuum. The residue obtained is purified by chromatography on silica gel, elution being carried out with a 70/30 heptane/ethyl acetate mixture. 3.7 g (66%) of methyl (R)-3-tert-butoxycarbonylamino-2-piperidin-1-yl-propanoate are obtained in the form of a light oil.

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.

Reference:
Patent; Clary, Laurence; Chambon, Sandrine; Chantalat, Laurent; Mauvais, Pascale; Roye, Olivier; Schuppli, Marlene; US2012/116072; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 628-77-3, 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. 628-77-3 name is 1,5-Diiodopentane, 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.

A solution of diiodopropane (19.0 g, 58.6 mmol) in THF (75 mL) was added dropwise over a period of 4 hours to a vigorously stirred solution of vanilic acid (20.0 g, 119 mmol) in THF (150 mL) and aqueous NaOH (340 mL) at 65 in the absence of light (foil-wrapped flask) . After heating at reflux for 48 hours in the dark, the solution was cooled and the THF removed by evaporation in vacuo. The residue was extracted with EA, The aqueous layer was separated and acidified to pH 2 with conc. HCl. The resultant precipitate collected by filtration, washed, dried and recrystallised from glacial acetic acid to afford the corresponding bis-carboxylic acid (14.0 g, 34.7 mmol) . White solid, yield (60%) ..

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,5-Diiodopentane, and friends who are interested can also refer to it.

Reference:
Patent; HANGZHOU DAC BIOTECH CO., LTD; ZHAO, Robert Yongxin; ZHUO, Xiaotao; YANG, Qingliang; ZHAO, Linyao; HUANG, Yuanyuan; YE, Hangbo; YANG, Chengyu; LEI, Jun; GAI, Shun; GUO, Huihui; JIA, Junxiang; BAI, Lu; XIE, Hongsheng; ZHOU, Xiaomai; GUO, Zhixiang; LI, Wenjun; CAO, Mingjun; ZHENG, Jun; YE, Zhichang; YANG, Yanlei; (325 pag.)WO2020/6722; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com