Tag: M.W=300-400

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. 364-11-4, name is 1-Bromo-4-iodo-2-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 364-11-4

General procedure: To a 20 mL vial with a stir bar was added aryl halide 1 (2.00 mmol), Pd(dba)2 (28.8 mg, 2.5 mol %), Xantphos (28.9 mg, 2.5 mol %). The vial was sealed with a Teflon-lined cap and THF (6.0 mL) was added. The mixture was vacuumed and backfilled with nitrogen (3×). A solution of ethyl 2-bromozincacetate (2a) in THF (0.40 M, 6.0 mL, 1.2 equiv) filtered through a Target Nylon 0.45 mum filter (1.25-inch OD) was syringed in and the reaction mixture was then heated to 65 C and monitored by HPLC. Upon reaction completion based on HPLC analysis (?95% conversion unless the reaction was stalled), the mixture was cooled to room temperature and quenched with 1 M aq HCl (5.0 mL), followed by addition of brine (5.0 mL). The organic layer was separated and concentrated in vacuum. The residue was purified by silica gel column chromatography using gradient EtOAc in hexanes.

The synthetic route of 364-11-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wong, Brian; Linghu, Xin; Crawford, James J.; Drobnick, Joy; Lee, Wendy; Zhang, Haiming; Tetrahedron; vol. 70; 7; (2014); p. 1508 – 1515;,
Iodide – Wikipedia,
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Reference of 628-77-3, 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. 628-77-3, name is 1,5-Diiodopentane, This compound has unique chemical properties. The synthetic route is as follows.

Example 15 (n=5); (a) 1, 1″- [ (Pentane-1, 5-diyl) dioxyjbisf (11S, llaS)-10- (tert- butyloxycarbonyl)-7-methoxy-11- (tetrahydro-pyran-2-yloxy)- 1, 2, 3, 10, 11, 11a-hexahydro-5H-pyrrolo [2, 1-c] [1, 4] benzodiazepine-5- one] (15c); 1,5-Diiodopentane (72.2 mg, 0.22 mmol, 0.5 equiv) was added to the mixture of monomer 14 (0.2 g, 0.44 mmol, 1.0 equiv) and potassium carbonate (0.98 mmol, 2.2 equiv) in dry DMF (30 mL), and the resulting mixture was heated to 90C under a nitrogen atmosphere for 5 h. Removal of excess solvent under reduced pressure afforded a crude solid, which was subjected to flash column chromatography (SiO2, 50% EtOAc-hexane) to afford the dimerized compound 15c (212 mg, 0.21 mmol, 98% yield, mixture of diastereomers from THP protecting group) as a solid: [a] 20D = +40 (c = 0.22, CHCl3) ; 1H NMR (CDC13, 400 MHz) : 5 1. 21-1. 83 (m, 64H, 14-H, Boc, THP), 1. 88-2. 18 (m, 24H, 1-H, 2-H, 13-H), 3.41-3. 73 (m, 16H, 3-H, 11a-H, THP), 3.84-4. 10 (m, 24H, 12-H, 7-OMe, THP), 4.97-5. 15 (m, 4H, THP), 5.66-5. 75 (d, 2H, 11-H), 5.77-5. 89 (d, 2H, 11-H), 6.50 (s, 2H, 9- H), 6.84 (s, 2H, 9-H), 7.17 (s, 2H, 6-H), 7.21 (s, 2H, 6-H); 13C NMR (CDCl3, 400 MHz): 6 19.9, 20.5, 21.0, 22.7, 23. 1, 23.3, 25.3, 28. 1, 28.2, 28.9, 29.1, 31.0, 31.3, 46.3, 56.0, 56.1, 60.0, 60.1, 63.4, 64.6, 68.7, 69. 0, 80. 9, 81. 3, 88.2, 91.2, 95.7, 100.4, 110.2, 110.7, 114.5, 115.0, 126.3, 129. 7, 129. 8, 148.5, 148.8, 150.0, 155.1, 167.4, 167.6 ; IR (neat): 3431,2945, 1704, 1643, 1604,1513, 1453, 1432, 1327,1271, 1202,1163, 1023cm-1 ; MS (FAB) m/z (relative intensity) 987 ([M + Na]+., 37), 965 (M +., 100), 763 (92), 863 (75), 982 (49).

The chemical industry reduces the impact on the environment during synthesis 1,5-Diiodopentane. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SPIROGEN LIMITED; WO2005/85259; (2005); A2;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 450412-29-0, name is 1-Bromo-3-fluoro-2-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 450412-29-0, Computed Properties of C6H3BrFI

Bromo-3-fluoro-2-iodobenzene (100 g, 333.5 mmol),5-Chloro-2-methoxyphenylboronic acid (62.2 g, 333.5 mmol) was dissolved in tetrahydrofuran (800 mL). To this was added a 2 M solution of sodium carbonate (500 mL)Tetrakis (triphenylphosphine) palladium (0) [Pd (PPh3) 4] (7.7 g, 6.7 mmol) was added and refluxed for 12 hours. After the reaction was completed, the mixture was cooled to room temperature, and the resulting mixture was extracted three times with water and toluene.The toluene layer was separated and dried over magnesium sulfate. The filtrate was distilled under reduced pressure, and the resulting mixture was recrystallized three times using chloroform and ethanol to obtain Compound A-1 (53.7 g, yield 51%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-3-fluoro-2-iodobenzene, and friends who are interested can also refer to it.

Reference:
Patent; LG Chem, Ltd.; Jeong Min-u; Lee Dong-hun; Huh Jeong-o; Jang Bun-jae; Huh Dong-uk; Han Mi-yeon; (48 pag.)KR2018/61075; (2018); A;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 19821-80-8, name is 1,3-Dibromo-2-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 19821-80-8, Product Details of 19821-80-8

50 g (138 mmol) of 1,3-dibromo-2-iodobenzene was added to a 1 L 3-neck round-And 1.3 g (6.9 mmol) of copper iodine,3.2 g (2.8 mmol) of Pd (PPh3) 4 is added and dissolved in 200 ml of triethylamine.After dissolving all the reactants, 17.5 g (171 mmol) of phenylacetylene was added under nitrogenSlowly add to the dropping funnel and stir at room temperature for 4 hours.After completion of the reaction, dilute 500 ml of normal hexane. Filter the reaction mixture into a Buchner vacuum funnel filled with 200 g of silica gel, remove the catalyst and salts, and wash with 1 L of n-hexane. The yellow oil is obtained by removing all the solvent of the filtered solution. (40 g, 86% yield)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Dibromo-2-iodobenzene, and friends who are interested can also refer to it.

Reference:
Patent; SFC Ltd.; Che Jong-tae; Choi Seong-geun; Kim Nam-i; Kim Hui-dae; (73 pag.)KR101923936; (2018); B1;,
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. 628-21-7, name is 1,4-Diiodobutane, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1,4-Diiodobutane

5 mol of 1,4-diiodobutane was dissolved in 5 L of a 35% acetone solution, the stirring speed was controlled at 150 rpm, 7 mol of 4-methyl-benzonitrile was added, the temperature of the solution was raised to 70 C, and the reflux was 110 min. , reduce the temperature of the solution to 15 C, filter, filter cake with a mass fraction of 55% methylamine solution, pour into the mass fraction of 27% potassium iodide solution layering, the oil layer is washed with sodium chloride solution, the mass fraction is 75% Washed with pentane solution, washed with 85% ethyl acetate solution, distilled under reduced pressure of 40 kPa, collected 55 C fraction, dehydrated with anhydrous sodium sulfate dehydrating agent to obtain finished productEthylene nitrile507.6 g, yield 94%.

According to the analysis of related databases, 628-21-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chengdu Dongdian Aier Technology Co., Ltd.; Yan Yida; (4 pag.)CN108264470; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 98-61-3, name is 4-Iodobenzenesulfonyl chloride, 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. Computed Properties of C6H4ClIO2S

General procedure: A: Sulfonyl chloride (1 eq.) was dissolved in a mixture of dry DCM (0.2 M) and TEA (1.5 eq.). Amine (1.2 eq.) was added and the reaction was stirred at 20 C until completion (TLC). The solvent was removed under reduced pressure and the crude product was purified by column flash-chromatography on silica to give the sulfonamide.

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

Reference:
Article; Heinrich, Daniel M.; Flanagan, Jack U.; Jamieson, Stephen M.F.; Silva, Shevan; Rigoreau, Laurent J.M.; Trivier, Elisabeth; Raynham, Tony; Turnbull, Andrew P.; Denny, William A.; European Journal of Medicinal Chemistry; vol. 62; (2013); p. 738 – 744;,
Iodide – Wikipedia,
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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. 147808-02-4, name is 2-Fluoro-1,4-diiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 2-Fluoro-1,4-diiodobenzene

Example 29 5-chloro-N-((1-(3-fluoro-4-(2-oxopyridin-1(2H)-yl)phenyl)-1H-imidazol-4-yl)methyl)thiophene-2-carboxamide (40) A mixture of 2,5-diiodofluorobenzene II-4 (2.50 g, 7.18 mmol), 4-hydroxymethylimidazole hydrochloride (0.967 g, 7.18 mmol), 8-hydroxyquinoline (0.104 g, 0.717 mmol) and K2CO3 (2.00 g, 14.5 mmol) in DMSO (12 mL) was degassed with Ar before being charged with CuI (0.136 g, 0.716 mmol). The mixture in a sealed tube was heated at 130 C. overnight. After being cooled to room temperature, H2O and EtOAc were added. It was filtered through celite. The organic phase was separated, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel column, eluted with MeOH in CH2Cl2 (0-5% MeOH) to give (1-(3-fluoro-4-iodophenyl)-1H-imidazol-4-yl)methanol (0.39 g).

The synthetic route of 147808-02-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Millennium Pharmaceuticals, Inc.; US2007/259924; (2007); A1;,
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 25252-00-0 as follows. Recommanded Product: 25252-00-0

Tetrahydrofuran (99.7g) and sodium borohydride (15.2g, 0.4mol) were added to the reaction flask at 10-25C.A solution of 2-bromo-5-iodobenzoic acid (109.4 g, 0.34 mol, prepared in Example 2) in tetrahydrofuran (151 g) was slowly added dropwise.At 10-30C, a solution of sulfuric acid (16.4 g) in tetrahydrofuran (25 g) was added dropwise to the reaction vessel. After the addition was completed, the reaction was performed at room temperature for 2 hours. Then, it was heated to reflux 66C, refluxed for 2 hours, and then lowered to room temperature. 5% hydrochloric acid (235 g) was slowly added dropwise and THF was distilled off under reduced pressure (-0.01 MPa).Add 326.7 g of MTBE and 222.7 g of water to dissolve the solid, cool to 15-25C, separate the layers, and evaporate the organic layer under reduced pressure (-0.095 MPa).Toluene (108.8 g) and water (108.8 g) were added and the mixture was warmed to 60C for 1 h, reduced to 18-22C and filtered. After drying, 89.1 g of an off-white solid product was obtained with a measured content of >99% and a yield of 85.1%.

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jinkai (Liaoning) Chemical Co., Ltd.; Wang Yongcan; Zhang Hong; Li Zhenwei; Zhao Yang; Zhang Guifang; Song Tongji; Hu Zhenzhu; Huang Fengting; (8 pag.)CN107954861; (2018); A;,
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 199850-56-1 as follows. Product Details of 199850-56-1

General procedure: To a solution of methyl 2-amino-4-chlorobenzoate (300 mg, 1.6 mmol) and ethyl 2-phenoxyacetate (320 mg, 1.8 mmol) in anhydrous THF (9 mL) was added KHMDS (4.8 mL, 1.0 M in THF, 4.8 mmol) in one portion with vigorous stirring under a nitrogen atmosphere. The reaction mixture was stirred at rt until completion of the reaction (10 min) then MeOH was added. The reaction mixture was concentrated under reduced pressure and the resulting residue was taken up in water and acidified with 1 N HCl until precipitation occurred. The precipitate was filtered, washed with EtOH then dried to give 7-chloro-4-hydroxy-3-phenoxyquinolin-2(1H)-one (Table 2, entry 1) as a pale pink powder (449 mg, 92%).

According to the analysis of related databases, 199850-56-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Toum, Jerome; Moquette, Alexandre; Lamotte, Yann; Mirguet, Olivier; Tetrahedron Letters; vol. 53; 15; (2012); p. 1920 – 1923;,
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. 249647-24-3, name is Methyl 3-bromo-4-iodobenzoate, A new synthetic method of this compound is introduced below., Formula: C8H6BrIO2

A solution of methyl 3-bromo-4-iodobenzoate (Preparation 23, 4.3 g, 12.6 mmol) in CH2Cl2 was cooled, under N2, to -78 C. DIBAL-H was added slowly to the solution, which was stirred at -78 C. for 45 minutes and then allowed to come to room temperature. Next, the reaction mixture was diluted with 1M HCL (40 mL) and stirred for 30 minutes. The reaction was further diluted with water and extracted with CH2Cl2. The organic phase was dried (Na2SO4) and concentrated under vacuum to afford the intermediate (3.2 g, 82%) as a solid. 1HNMR (CDCl3): 7.85 (1H), 7.67 (1H), 7.02 (1H), 4.65 (2H), 1.76 (1H, OH).

The synthetic route of 249647-24-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Vaillancourt, Valerie A.; Chubb, Nathan Anthony Logan; Curtis, Michael; Howson, William; Kyne, Graham M.; Menon, Sanjay; Sheehan, Susan M. K.; Skalitzky, Donald J.; Wendt, John A.; US2012/35122; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com