Tag: M.W=200-300

These common heterocyclic compound, 74534-15-9, name is 1-Chloro-2-iodo-4-nitrobenzene, 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. HPLC of Formula: C6H3ClINO2

The appropriate product 2 (1 mmol, 1 eq) in AcOH/EtOH (1:1, 0.42 M) was added slowly to a solution of Iron powder (6 eq) in AcOH/EtOH(1:2, 2 M) at 60C . The solution was stirred at 70C for 30-60 mins. The reaction mixture was cooled to 23C , filtered through celite, washed with ethyl acetate, and concentrated. The oily residue was dissolved in ethyl acetate (30 mL), washed with saturated aq. NaHCO3 (1 x 15 mL), water (2 x 10 mL), dried (MgSO4) and concentrated. The oily residue was used without further purification.

The synthetic route of 1-Chloro-2-iodo-4-nitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Fangying; Jiang, Hongxia; Deng, Yufang; Yu, Jiang; Zhan, Miao; Zhao, Lifeng; Chen, Yuanwei; Bioorganic and Medicinal Chemistry Letters; vol. 28; 14; (2018); p. 2399 – 2402;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

619-58-9, name is 4-Iodobenzoic acid, 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. category: iodides-buliding-blocks

248 mg (1 mmol) of 4-iodobenzoic acid and 720.54 mg (3 mmol) of sodium sulfide nonahydrate were added, copper powder 12.70 mg (0.2 mmol), ethanedithiol 8.4 uL (0.1 mmol) and 3 mL of solvent DMSO was placed in a 25 mL reaction tube equipped with a magnet, sealed with argon, heated and stirred, and reacted in an oil bath at 90 C for 12 hours. After completion of the reaction, the reaction solution was washed with NaOH solution and transferred to a 250 mL separatory funnel. The ether was extracted and the upper organic solvent was removed. The aqueous phase was adjusted to pH 1-3, extracted with dichloromethane and washed with water. Dried over magnesium sulfate. Evaporated under reduced pressure and subjected to column chromatography to afford 152 mg of product as a white solid, yield 99%

The synthetic route of 619-58-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dalian University of Technology; Liu Yajun; Xue Hongyu; Jing Bing; Liu Yong; (18 pag.)CN106916090; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile, 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 51628-12-7, Recommanded Product: 2-(4-Iodophenyl)acetonitrile

(1) A three-necked flask was added with p-iodobenzeneacetonitrile (0.04 mol), phloroglucinol (0.02 mol) and etherAgent, zinc chloride (0.012 mol) as a catalyst, HCl gas (30 ml) was bubbled in an ice-salt bath for 1 hour to observe the reactionThe medium should change from colorless to orange. The reaction was allowed to stand in the freezer for 12 hours, and then continued to pass HCl gas (25ml)1 hour, standing in the refrigerator for 2 days, remove the reaction solution, decanting ether, water bath heated to reflux for two hours, was recrystallizedTo 2,4,6-trihydroxy-4′-iodo-phenylbenzyl ketone of general formula IIa.

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; Nanhua University; Zheng Xing; Zheng Qutong; Wang Zongbao; Lei Xiaoyong; Zeng Xianliang; Xiao Yan; Liu Ya; Huang Qiuxia; (23 pag.)CN106432165; (2017); A;,
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. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., Formula: C3H6ClI

To a suspension of NaH (22 mg, 0.85 mmol) in DMF (2.0 mL) was added S1 (305 mg, 0.78 mmol) in DMF (1.5 mL). After 10 min at room temperature, S4a (0.20 mL, 1.53 mmol) was added to this mixture, and the reaction mixture was stirred at room temperature for 6 h, diluted with ether,washed with water and dried over Na2SO4. Purification by FCC (PE/EtOAc, 8 : 1) gave the chloride S5a (344 mg, 94%) as a yellow oil.

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; Gao, Yan; Shan, Dong; Jia, Yanxing; Tetrahedron; vol. 70; 34; (2014); p. 5136 – 5141;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 26670-89-3, 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. 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

2,6-Difluoro-N-(2′-methyl-5′-(pyridin-3-ylethynyl)biphenyl-4-yl)benzamide[00148] To the solution of 2-bromo-4-iodo-l-methylbenzene (0.3 g, 1.0 mmol) in TEA (4 mL) and toluene (1 mL) was added 3-ethynylpyridine (0.115 g, 1.12 mmol), CuI (0.04 g, 0.2 mmol), and Pd(PPh3)4 (0.065 g, 0.06 mmol). The resulting solution was heated at 1000C overnight before it was diluted with water and extracted with EtOAc (3chi20mL). The combined organic phases were dried and concentrated, and the column chromatography (Hexanes/EtOAc=l/l) afforded 2 in 66% yield. The desired compound was obtained from 2 through Suzuki coupling.[00149] 1H NMR (400 MHz, CDCb) delta 8.75 (d, / = 1.2 Hz, 1 H), 8.54-8.52 (m, 1 H), 7.81-7.78 (m, 1 H), 7.72-7.68 (m, 3 H), 7.45-7.43 (m, 3 H), 7.37-7.34 (m, 2 H), 7.29-7.27 (m, 2 H), 7.03 (t, / = 8.0 Hz, 2 H), 2.31 (s, 3 H); ESMS cacld (C27H18F2N2O): 424.1; found: 425.1 (M+H).

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-4-iodo-1-methylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SYNTA PHARMACEUTICALS CORP.; JIANG, Jun; ZHANG, Junyi; CHEN, Shoujun; SUN, Lijun; WO2010/39238; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, molecular formula is C8H9IO2, 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. Formula: C8H9IO2

Step 1: A mixture of I (117.0 g, 590 mmol), 4-iodo-1,2-dimethoxybenzene (85.0 g, 590 mmol), Pd(OAc)2 (13.2 g, 59 mmol) and tri(o-tolyl)phosphine (36.0 g, 118 mmol) in triethylamine (3 L) was heated at 90¡ã C. for 12 h. The mixture was cooled to room temperature and diluted with ethyl acetate (3 L). The organic phase was washed with brine, dried (MgSO4), and concentrated in vacuo to dryness. The crude product was purified by silica gel chromatography (0 to 40percent ethyl acetate/hexanes) to provide (1a) as a brown oil (87.0 g, 73percent based on the recovered starting material). 1H NMR (300 MHz, CDCl3): delta 6.85 (s, 2H), 6.79 (s, 1H), 6.64 (s, 1H), 3.98-3.93 (m, 4H), 3.88 (s, 3H), 3.86 (s, 3H), 2.10-2.00 (m, 4H), 1.81 (s, 3H), 1.68 (d, J=12.9 Hz, 4H), 1.17 (s, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5460-32-2, its application will become more common.

Reference:
Patent; Sequoia Sciences, Inc.; Williams, Russell B.; (17 pag.)US2017/73324; (2017); 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. 3718-88-5, name is 3-Iodobenzylamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., name: 3-Iodobenzylamine hydrochloride

Example 1 Preparation of N6 -(3-Iodobenzyl)-9-Methyladenine (3) A mixture of 6-chloropurine (1, 100 mg, 0.65 mmol), 3-iodobenzylamine hydrochloride (192 mg, 0.71 mmol), and triethylamine (0.27 mL, 1.94 mmol) in absolute ethanol (2 mL) was heated for 24 h at 80 C. After cooling, the resulting solid was filtered under suction, washed with ethyl acetate, and dried to give compound 2 (191.3 mg, 84.0%). 1 H NMR (DMSO-d6) delta 4.67 (br s, 2 H, CH2), 7.11 (pseudo t, J=7.6 and 7.5 Hz, 1 H, H-16), 7.37 (d, J=7.9 Hz, 1 H, H-17), 7.58 (d, J=7.6 Hz, 1 H, H-15), 7.73 (s, 1 H, H-13), 8.12 and 8.17 (each: s, 1 H, H-8 and H-2), 8.25 (br s, 1 H, exchangeable with D2 O, NH), 12.95 (br s, 1 H, exchangeable with D2 O, N9 H).

According to the analysis of related databases, 3718-88-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; The United States of America as represented by the Department of Health and Human Services; US5688774; (1997); A;,
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. 89459-38-1, name is 2-Iodo-4-nitrobenzoic acid, A new synthetic method of this compound is introduced below., Recommanded Product: 89459-38-1

Reference Example 82 2-Iodo-N-methoxy-N-methyl-4-nitrobenzamide An aqueous solution (8 ml) of sodium nitrite (2.27 g) was added to an aqueous solution (40 ml) of 4-nitroanthranilic acid (5.00 g) under ice-cooling. Subsequently, an aqueous solution (6 ml) of potassium iodide (5.47 g) was added to the mixture, followed by stirring at room temperature for 20 minutes, and then the mixture was heated to 75C, followed by further stirring for 10 minutes. After completion of the reaction, sodium hydrogen sulfite was added to the mixture under ice-cooling, and the mixture was extracted with dichloromethane-methanol (10:1, v/v). The organic layer was washed with water and saturated brine and dried over sodium sulfate. The residue obtained by evaporating the solvent was again dissolved in water and the same operation described in the above was repeated, and the thus obtained residue was used in the subsequent reaction without purification. The above-described residue was dissolved in dichloromethane, and N,O-dimethylhydroxylamine hydrochloride (3.21 g), HOBt (4.45 g), EDC-HCl (6.31 g) and N-methylmorpholine (3.6 ml) were added to the solution at 0C, followed by stirring overnight at room temperature. To the reaction solution was adde a saturated aqueous sodium bicarbonate solution, extracted with dichloromethane, washed with 1 N hydrochloric acid, water and saturated brine and dried over sodium sulfate. The solvent was evaporated, the thus obtained residue was purified by silica gel column chromatography, and the fraction obtained from the elude of n-hexane:ethyl acetate = 2:1 was concentrated under reduced pressure to obtain the title compound (6.57 g) as a colorless solid. 1H-NMR (400 MHz, CDCl3) delta: 3.41 (3H, s), 3.49 (3H, s), 7.44 (1H, d, J=8.5 Hz), 8.26 (1H, d, J=2.0 and 8.5 Hz), 8.67 (1H, d, J=2.0 Hz).

The synthetic route of 89459-38-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1612204; (2006); 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. 13194-68-8, name is 4-Iodo-2-methylaniline, A new synthetic method of this compound is introduced below., Computed Properties of C7H8IN

To a solution of 4-iodo-2-methyl-aniline (4.0 g, 17 mmol) and Pd (dppf) 2Cl 2 (140 mg, 0.17 mmol) in THF (50 mL) was added isopropylmagnisium chloride (25.5 mL, 51.0 mmol) at -78 and was reacted at reflux for 4 h. The reaction was quenched with a saturated solution of NH 4Cl, extracted with EtOAc, dried over anhydrous Na 2SO 4, filtered, and concentrated to dryness. The residue was purified by flash column chromatography to give the title compound as a brown solid (320 mg, 12%). MS (ESI) : mass calcd. for C 10H 15N, 149.1 m/z found, 150.0 [M+H] +.

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; JANSSEN PHARMACEUTICA NV; CAI, Min; ARORA, Nidhi; BACANI, Genesis M.; BARBAY, Joseph Kent; BEMBENEK, Scott D.; CHEN, Wei; DECKHUT, Charlotte Pooley; EDWARDS, James P.; GHOSH, Brahmananda; HAO, Baoyu; KREUTTER, Kevin D.; LI, Gang; TICHENOR, Mark S.; VENABLE, Jennifer D.; WEI, Jianmei; WIENER, John J. M.; WU, Yao; ZHU, Yaoping; ZHANG, Feihuang; ZHANG, Zheng; XIAO, Kun; (999 pag.)WO2018/103058; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 25245-27-6, 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. 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a 25 mL single-necked flask was added 3,5-dimethoxyiodobenzene (5 mmol)And pd (oAc) 2 (1.0 mol%) / Eosin Y (1.5 mol%)Dissolved in 6 mL DMF (DMF: H2O = 5: 1) aqueous solution,Then, p-hydroxystyrene (5.3 mmol) was slowly added dropwise,The reaction was stirred at room temperature for about 15 h,TLC detection reaction ends. The reaction product was washed with water, separated, dried,Filtered, concentrated, recrystallized from ethyl acetate,To obtain a white crystal, i.e. derivative 6a. the yield of 83.4%.

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-Iodo-3,5-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zhejiang University of Technology; Weng Jianquan; Dai Xiaoqiang; Zhu Yabo; Liu Xinghai; (7 pag.)CN106588582; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com