Author: Jessica.F

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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Iodo-2-(trifluoromethyl)benzene

General procedure: A mixture of aryl iodide (2 mmol), CuI (0.10 mmol), ligand(1.1 mmol), and S8 (1.1 mmol) were added to an oven-driedreaction tube equipped with a septum. The reaction tube wasevacuated and back-filled with argon. Under a counterflowof argon, EIPA (0.258 g, 2 mmol) and DMSO (2 mL) wereadded, and the mixture stirred at r.t. for 8 h. After completedisappearance of aryl iodide (monitored by TLC), H2O (5mL) was added, and the mixture was extracted with CH2Cl2(3 ¡Á 5 mL). The combined organic phases were dried (onMgSO4) and filtered before evaporation of the solvent. Theresidue was purified on silica gel, eluting with PE?EtOAc(20:1), to give product 2. Analytical and spectroscopic datafor all derivatives, except 2g?i have been reported previously.19

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yavari, Issa; Ghazanfarpour-Darjani, Majid; Solgi, Yazdan; Synlett; vol. 25; 8; (2014); p. 1121 – 1123;,
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. 144550-76-5, name is Methyl 2-amino-4-iodobenzoate, A new synthetic method of this compound is introduced below., Recommanded Product: Methyl 2-amino-4-iodobenzoate

e. Dimethyl 7-iodo-4-hydroxyquinoline-2,3-dicarboxylate Using a procedure similar to that described in Example 3c. except starting with methyl 2-amino-4-iodobenzoate, the crude title diester was obtained as a green solid (2.6 g, 92%). This material was purified by chromatography over silica gel (eluant: methylene chloride/methanol; 9.5/0.5) to provide the title compound (0.85 g, 30%) as a tan solid, mp 243-244 C.; MS(CI): 388 (M+H). Analysis for C13 H10 INO5: Calculated: C, 40.33; H, 2.60; N, 3.62 Found: C, 40.26; H, 2.77; N, 3.54

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; Imperial Chemical Industries, PLC; US5599814; (1997); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 82998-57-0,Some common heterocyclic compound, 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, molecular formula is C8H7IO2, 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.

3-iodo-4-methylbenzoic acid (3.2 g, 12.2 mmol) was dispersed in 50 mL of thionyl chloride.The reaction system was heated to 82 C, kept under reflux for 1 hour, and cooled to room temperature.The reaction solution was added to 50 mL of toluene while maintaining slow stirring.Concentrate under reduced pressure to a pale yellow oil.After the concentrate was dissolved in 100 mL of dichloromethane,To this solution was added 3-trifluoromethylaniline (2.3 mL, 18.3 mmol) and diisopropylethylamine (9 mL).The reaction system was stirred at room temperature overnight to precipitate a large amount of white solid.The reaction solution was concentrated under reduced pressure and then evaporated.Washed with saturated ammonium chloride solution and saturated brine,The organic phase was dried over anhydrous magnesium sulfate and concentrated.Purification by silica gel column chromatography to obtain compound 8(3.5 g, 71%) was obtained as a white solid.

The synthetic route of 82998-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shenzhen Ruixi Biological Technology Co., Ltd.; Jiao Zhaodong; Li Xitao; Tao Guanyu; Pan Zhengying; (36 pag.)CN109305944; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 755027-18-0, 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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

Step 1: 1-(4-Bromo-3-methoxyphenyl)-1H-pyrazol-3-amine A mixture of 1-bromo-4-iodo-2-methoxybenzene (2.5 g, 7.99 mmol), 3-aminopyrazole (0.797 g, 9.59 mmol), salicylaldoxime (0.219 g, 1.598 mmol), Cu2O (91 mg, 0.479 mmol), and Cs2CO3 (3.9 g, 11.98 mmol) in DMF (8 mL) was degassed with N2 and heated at 95 C. overnight. After cooling to RT, the mixture was filtered through celite and rinsed with EtOAc. The filtrate was washed with water and brine. The organic solution was dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by silica gel chromatography (10%-60% EtOAc in Heptane) to give 1-(4-bromo-3-methoxyphenyl)-1H-pyrazol-3-amine (800 mg, MS: 270.3 [M+H+]).

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

Reference:
Patent; NOVARTIS AG; AXFORD, Jake; DALES, Natalie; SUNG, Moo Je; US2014/206661; (2014); 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. 1094759-93-9, name is 4-Chloro-5-fluoro-2-iodoaniline, A new synthetic method of this compound is introduced below., Product Details of 1094759-93-9

To Intermediate 5 A (47g, 17.3 mmol) in AcOH (470 mL) was added NaN3 (33.76g, 51.9 mmol) and trimethyl orthoformate (56.8 mL, 51.9 mmol). After 30 h, the reaction was poured into ice water, then solid was filtered-off and washed with petroleum ether to afford 49 g of Intermediate 5B. MS (ESI) m/z: 324.8 (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; BRISTOL-MYERS SQUIBB COMPANY; ORWAT, Michael J.; PINTO, Donald J.P.; SMITH II, Leon M.; SRIVASTAVA, Shefali; WO2013/56034; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, 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

Example 8 Preparation of 3-(4-bromophenyl)-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole (C5) (0174) (0175) 3-(4-Bromophenyl)-1H-1,2,4-triazole (C4) (10.9 g, 48.5 mmol), copper(I) iodide (2.38 g, 12.5 mmol), and cesium carbonate (30.3 g, 93.0 mmol) in a round-bottomed flask was flushed with nitrogen. Dimethylsulfoxide (85 mL) was added, followed by 1-iodo-4-(trifluoromethoxy)benzene (13.2 g, 45.8 mmol). The reaction was degassed for 5 minutes, then heated at 100¡ã C. for 3 days. The reaction was cooled to room temperature, diluted with ethyl acetate, and filtered through a plug of Celite? rinsing with ethyl acetate. To the filtrate was added saturated ammonium chloride and stirred for 1.5 hours. The layers were separated and the aqueous layer was extracted with ethyl acetate (3¡Á). The combined organic layers were dried over magnesium sulfate, filtered, and concentrated onto Celite?. Purification by flash column chromatography using 0-40percent EtOAc/hexanes as eluent provided the title compound as an off-white solid (9.65 g, 52percent): mp 109-112¡ã C.; 1H NMR (400 MHz, CDCl3) delta 8.56 (s, 1H), 8.10-8.03 (m, 2H), 7.83-7.75 (m, 2H), 7.64-7.57 (m, 2H), 7.42-7.35 (m, 2H); ESIMS m/z 386 ([M+21-1 ]+).

The synthetic route of 103962-05-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DOW AGROSCIENCES LLC; Fischer, Lindsey G.; Crouse, Gary D.; Sparks, Thomas C.; Goldsmith, Miriam E.; Knueppel, Daniel I.; (66 pag.)US2016/24027; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 340825-13-0, A common heterocyclic compound, 340825-13-0, name is 6-Iodo-3,4-dihydronaphthalen-1(2H)-one, molecular formula is C10H9IO, 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.

In a tubular reactor, 6-iodolinone (81.6 mg, 0.3 mmol, 1.0 equiv.) And dimethyl sulfoxide (117.0 mg, 1.5 mmol, 5.0 equiv.) Were added in this order.And iodine (114.3 mg, 0.45 mmol, 1.5 equiv.),After being vacuumed and protected by nitrogen, it was placed at 80 C and stirred for 12 hours. After the reaction was completed,After cooling to room temperature, 5 mL of saturated aqueous sodium thiosulfate solution was added to the reaction mixture, and extracted 3 times with ethyl acetate (5 * 3 mL). Combine the organic phase,Dry with anhydrous sodium sulfate and spin-dry to obtain the pure product. The product separation yield was 85%.

The synthetic route of 340825-13-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xinyang Normal University; Ma Xiantao; Yu Jing; Fan Yu; Zhang Qian; Tang Lin; (10 pag.)CN111116436; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 144550-76-5, The chemical industry reduces the impact on the environment during synthesis 144550-76-5, name is Methyl 2-amino-4-iodobenzoate, I believe this compound will play a more active role in future production and life.

General procedure: (E)-3-(Naphthalen-2-yl)but-2-enoic acid (1.00 g, 4.71 mmol) was suspended in dry dichloromethane (15 mL) in a flame dried flask under an argon atmosphere and cooled to 0 C. Oxalyl chloride (0.848 g, 0.447 mL, 9.42 mmol) and a catalytic amount of DMF (2 drops) was added to the suspension and allowed to warm to room temperature. The solution was stirred at room temperature for 5 h after which all volatiles were removed under reduced pressure. The crude product was redissolved in dry dichloromethane (15 mL) and solvent removed under reduced pressure three times before drying under high vac. The crude product was redissolved in dry THF (20 mL) in a flame-dried flask under an argon atmosphere. To this was added 5-iodo-2-aminobenzoate (1.86 g, 7.07 mmol), pyridine (1.12 g, 1.14 mL, 14.1 mmol) and a catalytic amount of DMAP (0.01 g, 0.082 mmol). After stirring at 60 C for 16 h, the reaction was allowed to cool to room temperature, poured onto 1 N HCl and extracted into diethyl ether. The combined organic layers were dried over anhydrous magnesium sulphate and concentrated under vacuum to give the crude product.Purification by flash chromatography (8% methanolin dichloromethane) afforded the analytically pure product. (Yield:1.60 g, 3.39 mmol, 72%).

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, Methyl 2-amino-4-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Waghorn, Philip A.; Jackson, Mark R.; Gouverneur, Veronique; Vallis, Katherine A.; European Journal of Medicinal Chemistry; vol. 125; (2017); p. 117 – 129;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 64248-58-4,Some common heterocyclic compound, 64248-58-4, name is 1,2-Difluoro-4-iodobenzene, molecular formula is C6H3F2I, 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: PPh3 (1.3 mmol, 1.3 equiv), I2(1.3 mmol, 1.3 equiv) and4 cm3 toluene were added to a 20 cm3 test tube equipped witha stir bar, which was stirred for 10 min at room temperature.Then, aryl iodide 1, 4, or 5 (1 mmol), alkyne 2 (1.5 mmol,1.5 equiv), Pd(OAc)2 (3 mol%), and Et3N(5 mmol, 5 equiv)were added into the solution. At last, HCOOH (2 mmol, 2equiv) was added, and the tube was immediately sealed andstirred at 40 C for 4 h. After completion of the reaction,mixture was cooled to room temperature, filtered, and concentratedunder reduced pressure. The obtained residue waspurified by flash column chromatography on silica gel toprovide the corresponding products 3, 6, or 7.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,2-Difluoro-4-iodobenzene, its application will become more common.

Reference:
Article; Lyu, Xue; Sun, Guanglong; Zhou, Yang; Wang, Yingying; Lei, Min; Wu, Wanying; Guo, Dean; Monatshefte fur Chemie; vol. 150; 2; (2019); p. 309 – 315;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 19821-80-8, 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. 19821-80-8, name is 1,3-Dibromo-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 1,3-dibromo-2-iodobenzene of example 1 (13.7 g, 37.9 mmol, 1 eq) in tetrahydrofuran (160 mL) at -100 C. tert-butyllithium (75.9 mmol, 2 eq) in pentane (44.6 mL) was slowly added in the course of 3 h. After additional 1 h, 1,2-dibromobenzene (8.94 g, 4.57 mL, 37.9 mmol) was added dropwise and the reaction mixture was then allowed to reach 25 C. After 15 h, distilled water (150 mL) was added, followed by extraction with ethyl acetate (3¡Á150 mL). The combined organic layers were dried, filtered and evaporated. The residue was purified by flash chromatography which afforded 2,2′,6-tribromobiphenyl (12.9 g, 33 mmol, 97%) as white needles; m.p. 95-97 C.-1H NMR (400 MHz, CDCl3): delta=7.69 (1 H, d, J=8.1 Hz), 7.64 (2 H, dd, J=8.1, 0.7 Hz), 7.42 (1 H, tt, J=7.5, 0.9 Hz), 7.29 (1 H, ddt, J=7.8, 1.8, 0.7 Hz), 7.18 (1 H, dd, J=7.6, 1.6 Hz), 7.12 (1 H, dd, J=8.1, 0.7 Hz). -13C NMR (101 MHz, CDCl3): delta=142.2, 141.9, 132.6, 131.4, 130.6, 130.3, 129.8, 127.4, 124.4, 123.3. -C12H7Br3 (390.7): calculated C 36.87%, H 1.81%; found C 36.82%, H 1.66%.

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

Reference:
Patent; Leroux, Frederic; Bonnafoux, Laurence; Colobert, Francoise; US2010/137659; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com