Category: 624-76-0

These common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, 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. Application In Synthesis of 2-Iodoethanol

To a solution of compound 3 (2.00g, 6.43mmol) in acetone (20mL) was added potassium carbonate (1.33g, 9.64mmol), 2-iodoethanol (0.60mL, 7.72mmol) and stirred overnight at room temperature. After completion of the reaction, 120 water (150mL) and ethyl acetate (150mL) were added and the mixture was extracted with ethyl acetate twice. The combined extracts were washed with water (50mL×2) and brine (50mL×2), and dried over Na2SO4. After filtration, the solvent was removed under vacuum to obtain the crude compound. The crude compound was then purified by column chromatography on silica (60% EA/PE) to give compound 24 4 as a yellow oil (2.10g, yield 92.0%). 1H NMR (400MHz, CDCl3) delta 7.35 (s, 5H), 5.51 – 5.47 (m, 1H), 5.30 – 5.26 (m, 1H), 5.24 – 5.12 (m, 2H), 4.60 – 4.54 (m, 1H), 3.69 – 3.63 (m, 2H), 3.02 – 2.90 (m, 2H), 2.68 – 2.64 (m, 2H), 1.43 (s, 9H). 13C NMR (150MHz, CDCl3) delta 170.96, 155.46, 135.12, 128.76, 128.72, 128.62, 80.45, 67.63, 60.76, 53.77, 53.56, 36.29, 34.91, 28.39. ESI-MS: [M+Na]+ m/z 378.2

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

Reference:
Article; Du, Xinming; Qian, Jiawen; Wang, Yujie; Zhang, Mingming; Chu, Yiwei; Li, Yingxia; Bioorganic and Medicinal Chemistry; vol. 27; 13; (2019); p. 2784 – 2800;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 624-76-0, The chemical industry reduces the impact on the environment during synthesis 624-76-0, name is 2-Iodoethanol, I believe this compound will play a more active role in future production and life.

General procedure: A mixture of compound 1 (1 mmol) in acetonitrile (30 mL) and functionalized alkyl halides(1.3 mmol) was irradiated by ultrasound irradiation. The reaction was processed as described above togive the same ionic liquids 2-7.

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, 2-Iodoethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Rezki, Nadjet; Al-Sodies, Salsabeel A.; Shreaz, Sheikh; Shiekh, Rayees Ahmad; Messali, Mouslim; Raja, Vaseem; Aouad, Mohamed R.; Molecules; vol. 22; 11; (2017);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 624-76-0, These common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, 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: Conc. H2SO4 (0.3 equiv.) was added to 9-(4-methoxyphenyl)fluoren-9-ol (13) (1.0 equiv.) in toluene and warmed up to 60 C for 15 min. After cooling the solution to rt the corresponding hydroxyl alkyl halide (1.5 equiv) or the alkyldiol (2.0 equiv.) was added. The reaction mixture was stirred at rt for the given time and then partitioned between water and toluene. The organic phase was dried over MgSO4, filtered, and concentrated to dryness. The crude product was then purified by CC (iso-hexane/EtOAc = 9.5:0.5). 5.1.1.1 9-(2-Iodoethoxy)-9-(4-methoxyphenyl)-9H-fluorene (21) According to GP1: 9-(4-methoxyphenyl)fluoren-9-ol (13) [21] (1.4 g, 4.8 mmol), toluene (12 mL), conc. H2SO4 (147 mg, 1.50 mmol, 80.0 muL), 2-iodoethanol (14) (1.26 g, 7.35 mmol, 0.573 mL), 20 h. Yield: 2.0 g (92%); colourless solid, m.p. 96-98 C; TLC: Rf = 0.24 (iso-hexane/EtOAc = 9.5/0.5); IR (KBr): 3035, 2931, 2903, 2841, 2044, 1951, 1918, 1605, 1580, 1508, 1447, 1302, 1252, 1184, 1169, 1107, 1031, 993 cm-1; 1H NMR (CDCl3): delta = 3.15-3.20 (m, 2 H, CH2O), 3.20-3.24 (m, 2 H, ICH2), 3.75 (s, 3 H, CH3), 6.76-6.81 (m, 2 H, Har), 7.26 (td, J = 7.4/1.2 Hz, 2 H, Har), 7.29-7.32 (m, 2 H, Har), 7.33 (d, J = 7.4 Hz, 2 H, Har), 7.37 (td, J = 7.4/1.2 Hz, 2 H, Har), 7.66 (d, J = 7.4 Hz, 2 H, Har); 13C NMR (CDCl3): delta = 4.43 (t, 1 C, ICH2), 55.20 (q, 1 C, CH3), 63.93 (t, 1 C, CH2O), 88.42 (s, 1 C, CH2OC), 113.55 (d, 2 C, Car), 120.00 (d, 2 C, Car), 125.43 (d, 2 C, Car), 126.84 (d, 2 C, Car), 128.23 (d, 2 C, Car), 129.15 (d, 2 C, Car), 135.29 (s, 1 C, Car), 140.51 (s, 2 C, Car), 146.87 (s, 2 C, Car), 158.83 (s, 1 C, Car); MS (EI, 70 eV) m/z (%): 442 (30, M+), 271 (100); HRMS (EI, 70 eV): (C22H19IO2) calc. 442.0430, found 442.0475; Anal. C22H19IO2 (C, H, I, O).

The synthetic route of 624-76-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kerscher-Hack, Silke; Renukappa-Gutke, Thejavathi; Hoefner, Georg; Wanner, Klaus T.; European Journal of Medicinal Chemistry; vol. 124; (2016); p. 852 – 880;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 624-76-0, 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. 624-76-0, name is 2-Iodoethanol, This compound has unique chemical properties. The synthetic route is as follows.

Step C (1,1 -dimethylethyl)(2-iodoethoxy)dimethylsilane .OTBDMS Iodoethanol (2.68 kg, 15.4 mol), CH2CI2 (12 L) and imidizaole (1.556 kg, 22.63 mol) were chilled in an ice bath. A solution of t-butyldimethylchlorosilane (2.536 kg, 16.32 mol) in CH2CI2 (2.5 L) was added to the reaction over a 2 h period. The resulting white suspension was allowed to warm to rt over an 18 h. The reaction was worked up by washing with water and brine). The organic layer was dried (MgSC^) and evaporated under reduced pressure to provide the product of Step C as a light yellow oil. FontWeight=”Bold” FontSize=”10″ H NMR (400MHz, CDC13) delta = 3.75 (t, J = 7.0 Hz, 2 H), 3.11 (t, J = 7.0 Hz, 2 H), 0.77 – 0.89 (m, 10 H), 0.00 (s, 6 H).

The chemical industry reduces the impact on the environment during synthesis 2-Iodoethanol. I believe this compound will play a more active role in future production and life.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; WINTERS, Michael P.; BRANUM, Shawn; FAWZY, Nagy E.; KANG, Fu-An; REUMAN, Michael; RUSSELL, Ronald K.; SUI, Zhihua; TELEHA, Christopher A.; WO2013/152269; (2013); 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. 624-76-0, name is 2-Iodoethanol, A new synthetic method of this compound is introduced below., Product Details of 624-76-0

0.874 g (11.5 mmol) of thioacetic acid was placed in a 100 mL three-necked flask under N2 protection,(10.0 mmol) of 2-iodoethanol and 1.749 g (11.5 mmol) of DBU were slowly added dropwise to the reaction solution. After completion of the dropwise addition, the mixture was left to stand at room temperature After the reaction, the reaction product was passed through a silica gel column (the particle size of the silica gel was 200 to 300 mesh), and the filtrate was collected to give 0.5 g of a yellow oily liquid, i.e., a middle The yield was 42%.

The synthetic route of 624-76-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Liaoning University; Xia, Lin; Zhang, Aixia; Song, Peng; (14 pag.)CN104893710; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 624-76-0, name is 2-Iodoethanol, 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 624-76-0, Safety of 2-Iodoethanol

Acetone (4.0 mL) and sat. NaHCO3 aq. (20 mL) were added to a solution of compound 516 (300 mg, 0.640 mmol) in CH2Cl2 (6.0 mL). Then, a solution of Oxone (787 mg, 1.28 mmol) in H2O (10 mL) was dropwise added to this solution at 0 C. The reaction mixture was stirred at room temperature for 3 h. The resulting solution was extracted with CH2Cl2. The combined organic layer was washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue (310 mg) was dissolved in anhydrous CH2Cl2 (10 mL) under Ar atmosphere, then 2-iodoethanol (0.50 mL, 6.40 mmol) and ZnCl2 (1 M in THF, 0.64 mL, 0.64 mmol) was added to this solution at -78 C. The reaction mixture was stirred at 0 C for 1 h. After being quenched with sat. NaHCO3 aq. at 0 C, the mixture was filtered through a pad of Celite. The filtrate was diluted with EtOAc. The solution was washed with water and brine, dried over Na2SO4, and concentrated in vacuo. The residue (488 mg) was purified by column chromatography (silica gel 10 g, n-hexane: EtOAc = 5:1 to 2:1) to give a diastereomixture of 6 as a white powder (353 mg, 84%, 2 steps from 5).

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:
Article; Osawa, Takashi; Dohi, Masakazu; Hitomi, Yuka; Ito, Yuta; Obika, Satoshi; Hari, Yoshiyuki; Heterocycles; vol. 95; 1; (2017); p. 342 – 352;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 624-76-0, name is 2-Iodoethanol, 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 624-76-0, Product Details of 624-76-0

N-methylaniline (5mls, 0.05mol) was reacted with 2-Iodoethanol (3.599mls, 0.05mol) and diisopropylethylamine (8.039mls, 0.05mol) in ACN at 70oC for 16 hours. The solvent was evaporated and the residue was purified by silica gel column chromatography with hexane/EtOAc to provide the compound as a yellow orange oil (4.48g, 0.03mol, 64.5%yield). 1H NMR (400 MHz, Chloroform-d) delta 7.27 – 7.15 (m, 2H), 6.81 – 6.67 (m, 3H), 3.74 (t, J = 5.8 Hz, 2H), 3.42 (t, J = 5.8 Hz, 2H), 2.92 (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, 2-Iodoethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Bell-Horwath, Tiffany R.; Vadukoot, Anish K.; Thowfeik, Fathima Shazna; Li, Guorui; Wunderlich, Mark; Mulloy, James C.; Merino, Edward J.; Bioorganic and Medicinal Chemistry Letters; vol. 23; 10; (2013); p. 2951 – 2954;,
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 624-76-0 as follows. Quality Control of 2-Iodoethanol

A solution of 2-[(1-methylethyl)oxy]-5-[5-(1 ,2,3,4-tetrahydro-5-isoquinolinyl)-1 ,3,4- thiadiazol-2-yl]benzonitrile hydrochloride (Preparation 56) (50mg, 0.12 mmol) and potassium carbonate (50mg, 0.36 mmol) in DMF (1 ml) was treated with 2- iodoethanol (0.014ml, 0.18 mmol) and the mixture stirred at 8O0C for 2h. The mixture was diluted with water (10ml) and extracted with ethyl acetate (3x 10ml). The combined organic phases were dried (Na2SO4) and concentrated in vacuo. Purification of the residue by flash chromatography (cyclohexane/methanol: 0 to 5% gradient) gave 5-{5-[2-(2-hydroxyethyl)-1 ,2,3,4-tetrahydro-5-isoquinolinyl]-1 ,3,4- thiadiazol-2-yl}-2-[(1-methylethyl)oxy]benzonitrile (36mg, 71%) as a clear oil. LCMS (Method formate): Retention time 0.85min, MH+ = 421

According to the analysis of related databases, 624-76-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXO GROUP LIMITED; BAILEY, James, Matthew; BIT, Rino, Antonio; DEMONT, Emmanuel, Hubert; HARRISON, Lee, Andrew; JONES, Katherine, Louise; SMETHURST, Christian, Alan, Paul; WITHERINGTON, Jason; WO2010/146105; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 624-76-0, A common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, molecular formula is C2H5IO, 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.

1.5 equivalents of 2-iodoethanol was added to 2,3,3-trimethylindolenine and refluxed for 18 hours in toluene solvent to obtain intermediate 1. One equivalent of N, N’-diphenylformamidine and one equivalent of triethyl orthoformate was added to Intermediate 1 obtained, and refluxed in an ethanol solvent for 16 hours to obtain Intermediate 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:
Patent; Samsung SDI Co., Ltd; Lee Yeong; Kim Gyu-yeong; Choi Eun-jeong; Shin Myeong-yeop; Han Gyu-seok; (43 pag.)KR2018/76149; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 624-76-0, 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. 624-76-0, name is 2-Iodoethanol, This compound has unique chemical properties. The synthetic route is as follows.

2-Iodoethanol (467 muL, 6.00 mmol) was added to a solution of 2 (1.08 g, 3.00 mmol) and Cs2CO3 (3.04 g, 9.33 mmol) in DMF (10 mL) at 0 C. The reaction mixture was stirred for 9.5 h at 80 C, then the reaction was quenched with H2O, and the mixture was extracted with AcOEt. The organic layer was washed with H2O, dried over MgSO4, and concentrated. The resulting residue was purified by silica gel chromatography (hexane/AcOEt = 3/1) to give 3 (1.02 g, 2.51 mmol, 84%) as a white solid.

The chemical industry reduces the impact on the environment during synthesis 2-Iodoethanol. I believe this compound will play a more active role in future production and life.

Reference:
Article; Mita, Yusuke; Noguchi-Yachide, Tomomi; Ishikawa, Minoru; Hashimoto, Yuichi; Bioorganic and Medicinal Chemistry; vol. 21; 3; (2013); p. 608 – 617;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com