Month: January 2021

Adding a certain compound to certain chemical reactions, such as: 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, 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 391211-97-5, COA of Formula: C13H7F3INO2

Palladium hydroxide (100 mg) was suspended in a solution of l-(diphenylmethyl)-3-(2-hydroxyethyl)azetidin-3-ol (228 mg, 0.80 mmol) in methanol (15 mL), and the mixture was subjected to an atmosphere of hydrogen at 50 psi for 4 h. The catalyst was then removed by filtration through celite, and the filtrate was concentrated in vacuo to provide 3-(2-hydroxyethyl)azetidin-3-ol. This material was used in the subsequent reaction without purification. To a solution of 3,4- difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (314 mg, 0.80 mmol), prepared using procedures similar to those described in US 7,019,033, in DMF (4 mL) was added PyBOP (416 mg, 0.80 mmol) and triethylamine (223 muL, 1.6 mmol). Finally, the unpurified 3-(2-hydroxyethyl)azetidin-3-ol was added, and the resulting mixture was stirred at rt for 16 h. Water and ethyl acetate were added, and the layers were separated. The aqueous phase was extracted with once more with ethyl acetate. The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was purified by flash chromatography, eluting with ethyl acetate, to provide l-({3,4-difluoro-2-[(2-fluoro- 4-iodophenyl)amino]phenyl}carbonyl)-3-(2-hydroxyethyl)azetidin-3-ol as a colorless oil (303 mg, 0.62 mmol, 78% yield). 1H NMR (400 MHz, CDCl3): delta 8.46 (s, IH), 7.39 (dd, IH), 7.32 (m, IH), 7.13 (m, IH), 6.81 (m, IH), 6.60 (m, IH), 4.37 (br s, IH), 4.28 (br m, 4H), 3.94 (br s, 2H), 2.19 (br s, IH), 2.02 (m, 2H); MS (EI) for Ci8H16F3IN2O3: 491 (MH’).

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, 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; EXELIXIS, INC.; WO2008/76415; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, 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 2401-21-0, Recommanded Product: 2401-21-0

EXAMPLE 35 Benzyl 3-chloro-3-ethylsulphinyl-7-oxo-1-azabicyclo[3.2.0]heptane-2beta-carboxylate STR77 A solution of benzyl 3alpha-ethylthio-7-oxo-1azabicyclo[3.2.0]heptane-2beta-carboxylate (16) (0.050 g) in methylene chloride (5 ml) was stirred in an ice bath under argon and treated with water (1 drop), pyridine (0.040 g) and iodobenzene dichloride (0.091 g). The ice-bath was removed and the reaction mixture stirred at room temperature for 3 hours. The solution was then concentrated and chromatographed on silica gel 60 (<230 mesh) eluding with ethyl, acetate/60¡ã-80¡ã petroleum ether 7:3 to give benzyl 3-chloro-3-ethylsulphinyl-7-oxo-1-azabicyclo[3.2.0]heptane-2beta-carboxylate (56) (0.037 g) as a gum; tau(CDCl3) 2.61 (5H, s, phenyl), 4.75 (2H, s, benzyl CH2), 5.55 (1H, s, C2-H), 5.6-5.9 (1H, m, C5-H), 6.5-8.0 (6H, m, C4-H2, C6 -H2, SCH2) and 8.64 (3H, t J 7 Hz, CH3). This material was unstable and had to be progressed immediately as shown in example 17. 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; Beecham Group Limited; US4223038; (1980); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-44-8, 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. 626-44-8, name is 1,3,5-Triiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a mixture of 3-methoxy-6-(trimethylsilyl)ethynylpyridazine(0.185 g, 0.766 mmol), 1,3,5-triiodobenzene (0.100 g, 0.219 mmol), Pd2(dba)3(0.020 g, 0.021 mmol), CuI (0.004 g, 0.021 mmol), PPh3 (0.005 g, 0.021 mmol) under nitrogen atmosphere were added dry Et3N (10 mL) and toluene (10 mL). The reaction mixture was cooled to 0 C and TBAF (1 M in THF, 1.53 mL) was added dropwise and the reaction mixture was stirred for 10 min. The solution was heated to50C for 48 h. The reaction was cooled,filtered through Celiteandevaporated under reduced pressure. The crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate2:1) to give the title compound1as a brown solid (0.055 g, 55percent).

The synthetic route of 1,3,5-Triiodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Martin, Flavia-Adina; Baudequin, Christine; Fiol-Petit, Catherine; Darabantu, Mircea; Ramondenc, Yvan; Ple?, Nelly; Tetrahedron; vol. 70; 15; (2014); p. 2546 – 2555;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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: A mixture of substrate 1g (100.9 mg, 0.3 mmol), 2 (0.6 mmol), Pd(TFA)2 (10.0 mg, 10 mol%), TBHP (67.6 mg, 2.5 equiv) in DCE (2.0 mL) was charged in a glass sealed-tube and stirred under N2 atmosphere at 100 0C for 12 h. Upon completion of the reaction, saturated brine (15 mL) and dichloromethane (15 mL) were added to the mixture, then the aqueous layer was extracted with dichloromethane (15 mL ¡Á 2). The combined organic layer was dried over anhydrous MgSO4. Finally, the solution was concentrated in vacuo to provide a crude product, which was further purified via a column chromatography on silica gel (eluents: petroleum ether/ethyl acetate = 10:1) to supply the product 4.

The synthetic route of 696-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Miao-Miao; Shao, Ling-Yan; Lun, Li-Jun; Wu, Yu-Liang; Fu, Xiao-Pan; Ji, Ya-Fei; Chinese Chemical Letters; vol. 30; 3; (2019); p. 702 – 706;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 19099-54-8, 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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

In a dry 25 mL Schlenk reaction tube, 74 mg of 2-isopropyl iodobenzene, 203 mg of benzoic anhydride, 71 mg of benzoxazole, 5.3 mg of palladium chloride,14 mg of tris(2-furyl)phosphine, 43 mg of copper bromide, 56 mg of norbornene, 124 mg of potassium carbonate, and 3 mL of acetonitrile.Under nitrogen atmosphere, stirring was performed at 100C for 16 hours.After the reaction was completed, the mixture was cooled to room temperature and insoluble material was removed by filtration and passed through a silica gel column (volume ratio of ethyl acetate to petroleum ether was 1:10) to obtain 136 mg of a product in a yield of 40%. The reaction process was as shown in the following formula:

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

Reference:
Patent; Zhejiang University; Chen Wanzhi; Zhang Pingshun; Pan Shanfei; (24 pag.)CN107382894; (2017); 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3-Iodo-4-methylbenzoic acid

INTERMEDIATE 8; [2-methyl-5-(5-methyl-1 ,3,4-oxadiaz -2-yl)phenyl]boronic acid; a) Methyl 3-iodo-4-methylbenzoate; A suspension of 3-iodo-4-methylbenzoic acid (15.00 g, 60.00 mmol) and a 4M solution of hydrochloric acid in dioxane (20.00 mL, 80.0 mmol) in methanol (20 mL) was heated in a sealed tube at 80 C with stirring. After stirring for 3 days, the mixture was cooled and ethyl acetate and saturated aqueous potassium carbonate solution were added. The organic layer was washed with brine, dried (MgS04) and evaporated in vacuo to give the title compound (15.00 g, 95%).LR S (m/z): 277 (M+1)+.

According to the analysis of related databases, 82998-57-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALMIRALL, S.A.; AIGUADE BOSCH, Jose; CARRANCO MORUNO, Ines; WO2011/57757; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 877264-43-2,Some common heterocyclic compound, 877264-43-2, name is (5-Fluoro-2-iodophenyl)methanol, molecular formula is C7H6FIO, 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.

Step C: The product from Step B (6.2 g, 25.0 mmol) was dissolved in chloroform (170 mL) and the solution was added to a suspension of manganese (IV) oxide (43.0 g, 675 mmol) in chloroform (150 mL) and the mixture was stirred overnight at 75 C. The reaction mixture was filtered through a pad of diatomaceous earth and concentrated in vacuo to afford the desired product (3.7 g, 60% crude yield) as a yellow solid: 1H NMR (500 MHz, CDCl3) delta 10.01 (d, J=3.0 Hz, 1H), 7.92 (dd, J=8.7, 5.0 Hz, 1H), 7.60 (dd, J=8.6, 3.1 Hz, 1H), 7.10-7.06 (m, 1H).

The synthetic route of 877264-43-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Molino, Bruce F.; Liu, Shuang; Guzzo, Peter R.; Beck, James P.; US2006/52378; (2006); A1;,
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. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C8H9IO2

General procedure: An oven dried pressure tube was charged with haloarenes (0.5 mmol), copper(II) triflate (45 mg, 0.125 mmol), KNO2 (128 mg, 1.5 mmol) and anhydrous DMSO (0.6 mL) under nitrogen atmosphere. The tube was sealed with a teflon screw cap having mininert valve and nitrogen is purged through it for 5 min. It is stirred at room temperature for 10 min and then the temperature was gradually increased to 130 oC and is maintained at the same for 48 h. The reaction mixture was then cooled to room temperature, washed with excess ice cold water and extracted with ethyl acetate (3 x 10 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give the crude product which was purified by column chromatography using silica gel (Table 2, entries 1-18) or basic alumina (Table 2, entries 19-23) and a mixture of ethyl acetate and hexane as the eluent to afford the desired products in good yields.

The synthetic route of 16932-44-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Amal Joseph; Priyadarshini; Lakshmi Kantam; Maheswaran; Tetrahedron Letters; vol. 53; 12; (2012); p. 1511 – 1513;,
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. 75581-11-2, name is 4-Iodo-1-methoxy-2-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Safety of 4-Iodo-1-methoxy-2-methylbenzene

General procedure: Similar conditions for performing a Negishi coupling reaction with 15 have previously been described.4 A round bottom flask plus stir bar were dried and flushed with Ar before adding 1-iodo-3-isopropylbenzene (0.404 g, 1.64 mmol; purchased from Combi-Blocks) and anhyd. DMF (3 mL). Reaction was vacuum purged and refilled with Ar (3x) before the addition of Pd2dba3 (50 mg, 0.16 mmol) and P(o-tolyl)3 (75 mg, 0.082 mmol). A suspension containing organozinc 15 (5.5 mL, 2.5 mmol, 1.5 equiv.) was carefully added via syringe so as to avoid aspirating unreacted zinc metal. Reaction was stirred overnight at room temperature under Ar. Reaction mixture was quenched with sat. NH4Cl and extracted with EtOAc (2 x 15 mL). Organic phase was washed with brine, dried over MgSO4, filtered, concentrated and dried under high vacuum. Crude was purified by flash chromatography eluting with 5% EtOAc/Hexanes resulting in a beige solid: 277 mg (42%).

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 75581-11-2.

Reference:
Article; Augustyn, Evan; Finke, Karissa; Zur, Arik A.; Hansen, Logan; Heeren, Nathan; Chien, Huan-Chieh; Lin, Lawrence; Giacomini, Kathleen M.; Colas, Claire; Schlessinger, Avner; Thomas, Allen A.; Bioorganic and Medicinal Chemistry Letters; vol. 26; 11; (2016); p. 2616 – 2621;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 672-57-1, 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. 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To an oven-dried 25 mL ground mouth test tube equipped with a stir bar was added S-2-acetamidophenyl ethanethioate (0.5 mmol), 1-bromo-2-iodobenzene (0.6 mmol), Cs2CO3 (2.0 mmol), DMF (3 mL). The test tube was sealed with a sleeve rubber stopper and evacuated and refilled with argon for three cycles. The mixture was stirred 130 oC for 10 hours. After cooling to room temperature, the reaction mixture was quenched with water (20 mL), and extracted with ethyl acetate (20 mL) for three times. The combined organic layer was dried with anhydrous MgSO4, and condensed in vacuum on a rotary evaporator. The residual was purified on a silica gel chromatograph column by means of gradient elution (eluent: petroleum ether / ethyl acetate) to give the desired product.

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-Chloro-2-iodo-4-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhou, Yue; Zeng, Qingle; Zhang, Li; Synthetic Communications; vol. 47; 7; (2017); p. 710 – 715;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com