Month: March 2021

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. 624-75-9, name is 2-Iodoacetonitrile, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 624-75-9

General procedure: Starting amine (5.0 mmol) was dissolved in dry diethyl ether (17 mL) and iodoacetonitrile (5.5 mmol, 919 mg) was added dropwise under cooling. The mixture was stirred at room temperature for 3-14 days, then precipitate was filtered off, washed with diethyl ether and dried in vacuo to give the corresponding quaternary ammonium salt 2. If the solid precipitate was not formed after 7 days, the mixture was evaporated under reduced pressure. The crude product was washed with diethyl ether (3 ¡Á 15mL) and dried in vacuo. The quaternary ammonium salt 2 was used in the next step without additional purification. The corresponding quaternary ammonium salt (3.0 mmol) was heated at 150 C on oil bath in freshly distilled DMF (7 mL) in a 25 mL round-bottom flask fitted with reflux condenser and CaCl2-tube for 15 minutes. The mixture was cooled to room temperature, diluted with H2O (20 mL) and extracted with PhMe (2 ¡Á 15mL). The organic phase then was washed with H2O (2 ¡Á 15mL) and brine (15 mL), dried over Na2SO4 and evaporated in vacuo to give the desired aminoacetonitrile 4. The latter, if necessary, was purified by column chromatography (it is convenient to visualize aminoacetonitriles on TLC-plate by treating with the diluted solution of ninhydrin in EtOH). Note, that aminoacetonitriles are moisture sensitive. Products after column chromatography were additionally dried by the addition of dry PhMe (5 mL) and evaporation in vacuo.

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 624-75-9.

Reference:
Article; Buev, Evgeny M.; Smorodina, Anastasia A.; Stepanov, Maxim A.; Moshkin, Vladimir S.; Sosnovskikh, Vyacheslav Y.; Tetrahedron Letters; vol. 59; 17; (2018); p. 1638 – 1641;,
Iodide – Wikipedia,
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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. 88-67-5, name is 2-Iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2-Iodobenzoic acid

Weighing 5.52 g (20 mmol) of o-iodobenzoic acid ethyl ester obtained by esterification of o-iodobenzoic acid with anhydrous ethanol in a microwave reaction tube, 1.08 g (10 mmol) of o-phenylenediamine.Add copper iodide (190 mg, 1 mmol) in turn,Potassium phosphate (6.36g, 30mmol),Appropriate amount of ethylene glycol and magnetron at 180 C,Microwave reaction under nitrogen protection,The reaction was stopped after 1 h, and the reaction was terminated by TLC. Extraction with ethyl acetate (3 x 100 mL),Wash with water and an appropriate amount of saturated brine, combine the organic layers, add anhydrous Na2SO4 to remove water,After filtration, the residue was concentrated and the residue was purified by column chromatography to yield 1.The yield of the obtained Compound 1 was 65%.

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 88-67-5.

Reference:
Patent; Xinxiang Medical University; Yan Fulin; Cao Ke; Yan Jianwei; Ma Lijuan; Lv Haixia; Wang Yawen; Yin Tiantian; (25 pag.)CN108586364; (2018); A;,
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. 16355-92-3, name is 1,10-Diiododecane, This compound has unique chemical properties. The synthetic route is as follows., Formula: C10H20I2

Example 19: Preparation of C10-bis-L-Lactate Diol (Compound 19b) [0135] 25.0 g 1,10-diiododecane (Compound 18b) was dissolved in 7 ml DCM, and the solution added to 120 g tetrabutylammonium-L-lactate (Compound 17b). The reaction mixture was placed in a 40C rotary evaporator bath, and rotated at top speed for 20 hours. The solution was then diluted with 100ml dichloromethane, and washed with 100 ml water. 750 ml diethyl ether were placed into a 2-liter Erlenmeyer flask and stirred magnetically. The lower organic phase from the separatory funnel was dripped into the diethyl ether with stirring until a precipitate appeared. The precipitated salt (tetrabutylammonium iodide) was vacuum-filtered through a medium porosity frit, and the filtrate was collected in a 1-liter round-bottom flask and washed once with 400 ml 1.25% sodium thiosulfate in water, and twice with 400 ml water. The ether layer was dried over anhydrous magnesium sulfate and the solvent was removed in vacuo to produce 15.5 g of the product. [0136] The structure of the product was confirmed by’H NMR.

According to the analysis of related databases, 16355-92-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; POLYMERIX CORPORATION; RUTGERS, THE STATE UNIVERSITY OF NEW JERSEY; WO2005/39489; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C8H4F13I

Thiol No.1 was 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluoro-octane-1-thiol which was made as follows. Under nitrogen thiourea (1.1 equivalents) and 1-iodo-2-perfluorohexylethane (1 equivalent) were added to a degassed mixture of dimethoxyethane (DME, 9 parts) and water (1 part). The reaction mixture was held at reflux temperature for 8 hours. Most of the DME was distilled off and the distillation residue was allowed to cool to ambient temperature. Under stirring a solution of sodium methoxide in methanol (1 molar, 1.1 equivalents) was added to the suspension. Degassed water was added to the mixture. Thiol No.1 was collected quantitatively as the fluorous bottom layer.The spectroscopical data for the product were in agreement with those published elsewhere (J. Fluorine Chem. 1985, 28, 341-355 and J. Fluorine Chem. 1989, 42, 59-68).

The synthetic route of 2043-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPNAY; US2009/143608; (2009); 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. 14452-30-3, name is 1-(3-Iodophenyl)ethanone, A new synthetic method of this compound is introduced below., COA of Formula: C8H7IO

General procedure: General synthetic procedureof chalcones (2a-2y)Equimolar portions of theappropriately naphthaldehyde (20 mmol) and substituted acetophenone(20 mmol) were dissolved in approximately 80 mL of ethanol, stirring forseveral min at 0 C. Subsequently,10 mmolaliquot of 40% potassium hydroxide solution was added dropwise to the reactionflask. The reaction solution wasallowed to stir at room temperature from several hours to overnight, andthe precipitates were collected by filtration. Washed by cold enthanol (30 mL)for three times, the purified chalcones (2a-2y)were acquired.

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:
Article; Yan, Xiao-Qiang; Wang, Zhong-Chang; Li, Zhen; Wang, Peng-Fei; Qiu, Han-Yue; Chen, Long-Wang; Lu, Xiao-Yuan; Lv, Peng-Cheng; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry Letters; vol. 25; 20; (2015); p. 4664 – 4671;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 460-37-7, These common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, 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.

Example 1 2-Bromo-4-methyl-5-[(2,3,6-trifluorophenyl)[(3,3,3-trifluoropropyl)thio]methyl]pyridine Sodium hydride (60 mg, 1.38 mmol) and 1,1,1-trifluoro-3-iodopropane (165 mul, 1.38 mmol) were added to a N,N-dimethylformamide (5 ml) solution of (6-bromo-4-methylpyridin-3-yl)(2,3,6-trifluorophenyl)methanethiol (400 mg, 1.15 mmol) at 0 C., and the solution was stirred at room temperature for 2 hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed sequentially with water and saturated saline. The resulting organic layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was subjected to flash silica gel column chromatography (hexane/ethyl acetate) to give the title compound (390 mg, 0.878 mmol, 76%) as a yellow oil. 1H-NMR (400 MHz, CDCl3) delta: 2.23 (3H, s), 2.29-2.46 (2H, m), 2.65-2.77 (2H, m), 5.48 (1H, s), 6.84-6.90 (1H, m), 7.08-7.16 (1H, m), 7.28 (1H, s), 8.79 (1H, s). MS (m/z): 444 (M++H).

Statistics shows that 1,1,1-Trifluoro-3-iodopropane is playing an increasingly important role. we look forward to future research findings about 460-37-7.

Reference:
Patent; DAIICHI SANKYO COMPANY, LIMITED; US2010/168136; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 42861-71-2, These common heterocyclic compound, 42861-71-2, name is 3-Iodophenyl acetate, 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 stirring solution of 3-iodo phenyl acetate (32.20 g, 123 mmol) in chlorobenzene (250 ml) under nitrogen was added aluminium chloride (31.00 g, 232 mmol, 1.9 equ). The reaction mixture was heated to [140C] for 90 hours then allowed to cool. The reaction mixture was poured onto ice/water and then filtered, and the residue washed with dichloromethane. The filtrate was then extracted with dichloromethane and the combined organic layers extracted with 10 [%] potassium hydroxide solution (3x 100 ml). The combined aqueous layers were then acidified with 6N hydrochloric acid and extracted with dichloromethane (3x 75 ml). This organic layer was then dried (MgSO4) and concentrated in vacuo to give 29 (22.3 g, 69 %) as a brown solid. [1H] nmr (400 MHz, [CDC13).] 2.60 (s, 3H) 7.26-7. 28 (m, [2H)] 7.42 (s, 1H) [12.] 26 [(S,] [1H). 13C] nmr (100 MHz, CDCl3) 26.596 [(CH3),] 103.768 (Q), [118. 997] (Q), 127. 833 (CH), 128.325 (CH), 131.251 (CH), 162.191 (Q), 204.214 (Q). CI+ 263.0 [(98] %, M+H+) 262 [(100%,] [M+). ACC. MASS.] (M+H) [CUSDH8O2I,] calc. 262.9569, found 262.9568. ir (GG) 2360g 1699g 1558g 1205. mp. 51.5- [52C] (lit. [52-54C*).]

The synthetic route of 42861-71-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ROWETT RESEARCH INSTITUTE; WO2004/7475; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 249647-24-3, name is Methyl 3-bromo-4-iodobenzoate, 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 249647-24-3, Recommanded Product: 249647-24-3

A solution of the compound obtained in 81-1 (5.02 g, 29.771 mmol) in THF (35 mL) was added with 9-BBN (0.5M THF solution, 65.5 mL, 32.748 mmol) and stirred at room temprature for 2.5 hours. The mixture was added with DMF (100 mL), methyl 3-bromo-4-iodobenzoate (11.17 g, 32.748 mmol) and K2CO3 (12.34 g, 89.313 mmol), and then substituted with nitrogen for a few minutes. Then, the mixture was added with Pd(dppf)Cl2¡¤MC (1.22 g, 1.489 mmol) and allowed to react at 100C for 16 hours. After cooled to room temperature, the reaction mixture was added with distilled water and brine, and then extracted with EtOAc. The organic layer was collected and dried over MgSO4. The filtrate thus obtained was concentrated under reduced pressure and purified by silica gel chromatography to obtain the title compound (yellow oil, 5.38 g, 47% yield). 1H NMR (300 MHz, CDCl3) delta 8.20 (d, 1H), 7.90 (dd, 1H), 7.29 (d, 1H), 6.98 (s, 1H), 3.92 (s, 3H), 2.90 – 2.74 (m, 4H), 2.50 (s, 3H), 2.17 – 1.99 (m, 2H).

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; SK Chemicals Co., Ltd.; LEE, Ju Young; LEE, Jeong A; AHN, Jaeseung; RYU, Je Ho; HAN, Min-Young; YOO, Taekyung; SA, Joon Ho; KIM, Jae-Sun; (297 pag.)EP2963027; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 167479-01-8, The chemical industry reduces the impact on the environment during synthesis 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate, I believe this compound will play a more active role in future production and life.

Example 38; tert-Butyl r3-r{6-methoxy-4-r(2-methyl-5-{J3-(trifluoromethv?benzoyl]aminolphenv? amino]quinazolin-7-yl>oxy)propyl]carbamate; A solution of N- {3-[(7-hydroxy-6-methoxyquinazolin-4-yl)amino]-4-?iethylphenyl} -3-(trifluoromethyl)benzamide (Example 70; 100 mg, 0.213 mmol), tert-butyl (3- iodopropyl)carbamate (Method 26; 61 mg, 0.213 mmol, 1.2 equiv) and K2CO3 (44 mg, 0.320 mmol, 1.5 equiv) in MeCN (2 ml) were heated to 70 0C for 12 h. The reaction was quenched with water and extracted with EtOAc. The organics were dried with nuaCl(sat) and Na2SO4(S) and then removed under reduced pressure. The resulting solid was purified by reverse phase preparative HPLC (0.1% TFA in MeCN and water); m/z 626.

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, tert-Butyl (3-iodopropyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2007/71963; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 58755-70-7, A common heterocyclic compound, 58755-70-7, name is 1-Iodo-4-methoxy-2-nitrobenzene, molecular formula is C7H6INO3, 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.

K3PO4 (5.09 g, 24.0 mmol) and PdCl2(dppf)¡¤CH2Cl2 (327 mg, 0.400 mmol) was added to a solution of 4-iodo-3-nitroanisole (33, 2.28 g, 8.00 mmol) and 8 (2.18 g, 8.80 mmol) in DMF (30 ml) and water (0.6 ml) under argon atmosphere, and the mixture was stirred for 3 h at 70 C. The reaction mixture was filtered through Celite, and the filtrate was diluted with water, extracted with methylene chloride. The organic layer was washed with water and brine, dried with sodium sulfate, and evaporated. The residue was purified by silica gel column chromatography (n-hexane/ethyl acetate 15:1 to 10:1) to give 34 (orange solid, 1.78 g, 6.52 mmol, 81%). Mp 137.5-138.0 C; 1H NMR (500 MHz, CDCl3) delta 7.43 (d, 1H, J=2.6 Hz), 7.28 (d, 1H, J=8.5 Hz), 7.15 (d, 1H, J=7.7 Hz), 7.14 (dd, 1H, J=8.5, 2.7 Hz), 6.87 (d, 1H, J=7.6 Hz), 6.71 (s, 1H), 3.87 (s, 3H), 3.67 (s, 3H), 2.39 (s, 3H); 13C NMR (125 MHz, CDCl3) delta 158.81, 155.73, 150.04, 139.58, 133.23, 129.35, 125.19, 123.94, 121.76, 118.85, 111.55, 108.94, 55.78, 55.00, 21.61; HRMS (FAB+) m/z 274.1075 [(M+H)+: calcd for C15H16NO4, 274.1079].

The synthetic route of 58755-70-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Iwashita, Masazumi; Fujii, Shinya; Ito, Shigeru; Hirano, Tomoya; Kagechika, Hiroyuki; Tetrahedron; vol. 67; 33; (2011); p. 6073 – 6082;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com