Author: Jessica.F

Related Products of 58313-23-8,Some common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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.

A -45 C. solution of ethyl 3-iodobenzoate (2.434 g, 8.8 mmol) in 40 mL THF was treated with i-PrMgCl (4.8 mL, 9.6 mmol, 2 M/ether). After 1 h, allyl bromide (1.6 mL, 18.9 mmol) was added followed by CuCN (79 mg, 0.88 mmol). The reaction was stirred for 1 h and then was quenched by addition of 50 mL saturated NH4Cl solution. Water (30 mL) was added and the resulting mixture was extracted with ethyl acetate (3*50 mL). The combined ethyl acetate solution was dried (MgSO4), filtered and evaporated. Purification by flash chromatography on silica gel (5% ethyl acetate/hexanes?10%) gave compound 7 (1.145 g, 68%).

The synthetic route of 58313-23-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALLERGAN, INC.; US2009/239869; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 216393-67-8, A common heterocyclic compound, 216393-67-8, name is 4-Chloro-2-fluoro-6-iodoaniline, molecular formula is C6H4ClFIN, 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 mixture of 3-ethynylpyridine (1.13 g, 11 mmol) and 2-fluoro^-chloro-6-iodoaniline (2.71 g, 10 mmol) in triethylamine (100 mL) is added PdCI2(PPh3)2 (175 mg, 0.25 mmol) and CuI (95 mg, 0.50 mmol) and the mixture is refluxed for 1 h. The solvent is removed in vacuo and the residue is purified by silica gel flash chromatography (dichloromethane- methanol, 1 :0 to 24:1 ) to give 4-chloro-2-fluoro-6-pyridin-3-ylethynyl-phenylamine. MS (ESI) m/z 247 (M+H)+.

The synthetic route of 216393-67-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; WO2009/156462; (2009); A2;,
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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H6BrIO2

General procedure: 500mL round-bottom flask reactor, methyl 5-bromo-2-iodo benzoate (25.0g, 73mmol) in 4-dibenzofuran boronic acid(18.7g, 88mmol), tetrakis (triphenylphosphine) palladium (1.7g, 0.15mmol), potassium carbonate (20.2 g,Put 146.7mmol) were placed 125 mL toluene, tetrahydrofuran, 125mL, water 50 mL. The temperature of the reactor 80 road winsOn and stirred 10 hours. When the reaction is complete cool down the temperature of the reactor to room temperature, extracted with ethyl acetate and the organicAnd separating the base layer. The organic layer was obtained an intermediate a-1 (75.0g, 60.1%) and, after concentration under reduced pressure, separated by column chromatography. Synthesis Example 1- (1) in the 4-dibenzofuran boronic acid, except that instead of the and is, using the same method to give the (8.2g, 68.6%) .

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; SFC CO., LTD.; CHA, SUN OK; JONG, KYONG SEOK; SONG, JOO MIN; LEE, YU RIM; PARK, SANG WOO; KIM, HUI DAE; PARK, SEOK BAE; (76 pag.)KR2016/13678; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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

Synthetic Route of 3819-88-3, A common heterocyclic compound, 3819-88-3, name is 1-Fluoro-3-iodo-5-nitrobenzene, molecular formula is C6H3FINO2, 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 solution of 1.0 eq IA in dry DMF (0.37 M) was added Zn(CN)2 (0.92 eq) and Pd(PPhj)4 (0.058 eq). The reaction mixture was purged with nitrogen and heated to 800C overnight. An additional 0.023 eq of Pd(PPh3)4 was then added and the reaction was heated for another 6 hrs. The reaction mixture was then cooled to RT, diluted with 15 volumes of EtOAc (based on IA) and the organic layer was washed 3 times with water and once with brine. The organic layer was dried over sodium sulfate, filtered and concentrated. Purification by chromatography over silica, gel using 10% Et2O/hexane as the eluant provided IB as a solid (90%).

The synthetic route of 3819-88-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CYTOKINETICS, INC.; WO2007/70683; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 191348-14-8, name is 2-Iodo-4-methoxyaniline, 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 191348-14-8, Recommanded Product: 191348-14-8

General procedure: Step B: Pyridine (1.5 mmol) was added to the o-iodo derivative as prepared above (1 mmol) in DCM (5 mL) at 0 C under nitrogen atmosphere. To this was added methane/p-toluene sulfonyl chloride (1.2 mmol) slowly at 0 C. Then, the reaction mixture was stirred at room temperature for 5-6 h. After completion of the reaction (monitored by TLC), the reaction mixture was diluted with ethyl acetate (30 mL), washed with 2N HCl solution (10 mL) followed by brine solution (20 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography using ethyl acetate-hexane to give the desired product 2.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Iodo-4-methoxyaniline, and friends who are interested can also refer to it.

Reference:
Article; Rambabu; Raja, Guttikonda; Yogi Sreenivas; Seerapu; Lalith Kumar; Deora, Girdhar Singh; Haldar, Devyani; Rao, M.V.Basaveswara; Pal, Manojit; Bioorganic and Medicinal Chemistry Letters; vol. 23; 5; (2013); p. 1351 – 1357;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 7681-82-5,Some common heterocyclic compound, 7681-82-5, name is Sodium iodide, molecular formula is INa, 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 solution of complex [Pd(P,P)Cl2] (100 mg, 0.138 mmol) in10 mL of acetone, were added 207 mg of NuaI (1.380 mmol), underinert atmosphere and vigorous stirring. The dark yellow solutionwas stirred at room temperature for 2 h. After acetone wascompletely removed under vacuum, 10 mL of CH2Cl2 were addedto the resulting solid. The mixture was filtered in order to removethe inorganic salts. Subsequent addition of n-hexane (20 mL) to thefiltrate led to the formation of a yellow solid, which was filteredand dried under vacuum. Yield: 103 mg, 82%. HRMS (positiveESI-MS, Fig. S1, Supplementary Material): calcd for C30H35I2NNaO3P2PdSi [M+Na]+ 929.8878, found 929.8898; calcd forC30H35I2KNO3P2PdSi [M+K]+ 945.8617, found 945.8634. IR (KBr,cm1): 513 (s), 558 (m), 693 (s), 741 (s), 869 (s), 1098 (s), 1430(s), 2820 (w), 2931 (w). 1H NMR (300 MHz, CDCl3): d 0.20 (t, 2H,Si-CH2), 1.20 (m, 2H, -CH2-CH2-Si), 1.60, 2.80 (m, 2H, N-CH2),3.40 (s, 9H, Si-OCH3), 7.30, 7.4-8.0 (m, 20H, Harom). 31P NMR(121.5 MHz, CDCl3): d 24.2. UV-Vis (CH2Cl2), [k (nm), e (M1cm1)]: (418, 6800), (292, 23000), (263, 26150).

The synthetic route of 7681-82-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Stamatopoulos, Ioannis K.; Kapsi, Maria; Roulia, Maria; Vougioukalakis, Georgios C.; Raptopoulou, Catherine P.; Psycharis, Vassilis; Kostas, Ioannis D.; Kollar, Laszlo; Kyritsis, Panayotis; Polyhedron; vol. 151; (2018); p. 292 – 298;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
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. 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, A new synthetic method of this compound is introduced below., Safety of 1,3-Difluoro-5-iodobenzene

PotassI.um phosphate (1.9 g, 8.7 mmol), trI.s(dI.benzylI.deneacetone)dI.palladI.um (0.27 g, 0.29 mmol), Xantphos (0.17 g, 0.29 mmol) and 3,5-dI.fluoroI.odobenzene (1.5 g, 6.4 mmol) were addedsuccessI.vely to a mI.xture of ethyl 2-aminothI.azole-4-carboxylate (1.0 g, 5.8 mmol) I.n a mI.xture of 9 ml of toluene and 3 ml of water. The mI.xture was flushed wI.th argon for 20 mins, then heated I.n the mI.crowave to 140 C for 1 h. The reactI.on mI.xture was dI.luted wI.th water and extracted wI.th ethyl acetate. The organI.c layer was washed wI.th saturated aqueous sodI.um bI.carbonate solutI.on and water, drI.ed over magnesI.um sulfate and evaporated under reduced pressure. The resI.due was purI.fI.ed bychromatography on sI.lI.ca gel, usI.ng ethyl acetate and cyclohexane as eluents, to delI.ver ethyl 2-(3,5- dI.fluoroanI.lI.no)thI.azole-4-carboxylate (0.16 g, 0.56 mmol). 1H-NMR (400 MHz, CDCl3): oe = 1.41 (t, 3H), 4.40 (q, 2H), 6.54 (t, 1H), 6.95 (d, 2H), 7.63 (s, 1H)

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; SYNGENTA PARTICIPATIONS AG; JEANMART, Stephane, Andre, Marie; ZAMBACH, Werner; RENDINE, Stefano; LAMBERTH, Clemens; BEAUDEGNIES, Renaud; POULIOT, Martin; BONVALOT, Damien; (73 pag.)WO2017/207362; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com