Tag: M.W=200-300

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. 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C8H8INO2

4-Amino-3-iodo-iV,./V-dimethylbenzamide < To a stirred solution of dimethylamine (9.0 mL, 135 mmol) in THF at O0C was added trimethylaluminium (50 mL, 2.0M solution in toluene, 100 mmol). The resulting solution was stirred at 00C for 10 minutes before addition of a solution of methyl 4- amino-3-iodobenzoate (19 g, 70 mmol) in THF (50 mL). The solution was heated to reflux for 1.5 h then allowed to cool to r.t before being poured onto ice (100 g). The resulting suspension was treated with aqueous 2M NaOH solution (100 mL) and partitioned with diisopropyl ether (2 x 100 mL). The combined organics were passed through a phase separator and concentrated to give the title compound (20 g, 96%) as a pale yellow oil which was used without further purification. 5H (CDCl3) 7.79 (IH, d, J 1.5 Hz), 7.29-7.26 (IH, m), 6.72 (IH, d, J8.2 Hz), 4.31 (2H, br. s), 3.07 (6H, s). LCMS (ES+) 261 (M+H)+.

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 19718-49-1.

Reference:
Patent; UCB PHARMA S.A.; WO2009/71888; (2009); A1;,
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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, category: iodides-buliding-blocks

To a solution of 2-iodo-4-methoxyaniline 30-d ( 1.00 g, 4.02 mmol) in DMF cooled to 0C were sequentially added diethylamine (41 uL, 4.02 mmol), copper(I) iodide ( 143 mg, 0.80 mmol) and dichlorobis(triphenylphosphine) palladium (II) (282 mg, 0.40 mmol). After complete dissolution of copper(I)iodide, propyl 3,3-dimethylhex-5- ynoate 1 1 -d (805 mg, 4.42 mmol) was added dropwise at 0 C and the reaction was then stirred at room temperature overnight. Water and ethyl acetate were added; the organic layer was separated, washed with saturated aqueous ammonium chloride and brine, dried over anhydrous MgS04, filtered and concentrated in vacuo. Purification by silica gel chromatography provided intermediate 30-e as a beige oil. MS (m/z) M+H=3()4.4

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, 2-Iodo-4-methoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AEGERA THERAPEUTICS INC.; BUREAU, Patrick; FOURNIER, Jean-Hugues; JAQUITH, James, B.; LAURENT, Alain; ROSE, Yannick; PROULX, Melanie; WO2011/35417; (2011); A1;,
Iodide – Wikipedia,
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Related Products of 90347-66-3,Some common heterocyclic compound, 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, 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.

3-iodo-4-methylbenzoic acid. Methyl-3-Iodo-4-methylbenzoate (3 g, 109 mmol, 1 eq) dissolved in MeOH (30 ml) was added sodium hydroxide (1.3 g, 327 mmol, 3 eq) followed by the addition of water (15 ml). The above solution was stirred at room temperature for 14 h. The solution was concentrated under vacuum, and then added water. The pH of the reaction was bought to 3 using Cone. HCl. The solid obtained was filtered and dried under vacuum, Yield: 2.7 g (96 %). 1HNMR (400MHz, DMSO-d6): delta 2.44 (s, 3H), 7.45 (d, 7- 8.00 Hz ,1H), 7.85 (d, J= 3.18 Hz, IH), 8.31 (s, IH).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 3-iodo-4-methylbenzoate, its application will become more common.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; PRACITTO, Richard; KADOW, John F.; BENDER, John A.; BENO, Brett R.; GRANT-YOUNG, Katharine A.; HAN, Ying; HEWAWASAM, Piyasena; NICKEL, Andrew; PARCELLA, Kyle E.; YEUNG, Kap-Sun; CHUPAK, Louis S.; WO2010/30538; (2010); A2;,
Iodide – Wikipedia,
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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. 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

Methyl 4-formyl-3-methylbenzoate (1616-18a). To a solution of methyl 4-iodo-3- methylbenzoate (1.0 g, 3.6 mmol) in THF (24 mL, 0.15 M) at -15C was added isopropylmagnesium chloride (7.2 ml, 14.5 mmol, 4.0 equiv). The reaction mixture was allowed to continue stirring at -15C for 2 hrs before N,N-dimethylformamide (1.4 ml, 18mmol, 5.0 equiv) was added. The mixture was warmed to room temperature over a period of 1 hr. At this time the reaction was quenched with HC1 and extracted with EtOAc (3x). The combined organic layers were washed with brine and dried over MgSO4, filtered and concentrated in vacuo.Purification was achieved using flash column chromatography on Si02 (Hexanes/EtOAc:6/1) to yield a white solid (0.45 g, 70 %) which was taken on without further purification.

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; EMORY UNIVERSITY; TRAYNELIS, Stephen F.; MULLASSERIL, Praseeda; GARNIER, Ethel C.; LIOTTA, Dennis C; ZIMMERMAN, Sommer; WO2014/25942; (2014); A1;,
Iodide – Wikipedia,
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Electric Literature of 128140-82-9, The chemical industry reduces the impact on the environment during synthesis 128140-82-9, name is 1-(Difluoromethoxy)-4-iodobenzene, I believe this compound will play a more active role in future production and life.

Step 1) 1-((4-(Difluoromethoxy)phenyl)ethynyl)-3-methylbenzene To a solution of 3-bromophenylacetylene (2.5 g, 21.5 mmol), TEA (9.57 g, 94.6 mmol, 13.2 mL), bis(triphenylphosphine)dichloropalladium(II) (603 mg, 0.86 mmol), and CuI (98 mg, 0.516 mmol) in DMF (26 mL) was added 4-iodo(difluoromethoxy)benzene (4.64 g, 17.2 mmol) at room temperature. The reaction mixture had gotten warm after the addition was completed. The mixture was stirred for 4 h then the mixture was portioned between EtOAc and water. The aqueous layer was separated and extracted twice with EtOAc. The combined organic layers were dried over Na2SO4, filtered, and concentrated over 20 g Celite. Flash chromatography (SiO2, Hexanes) gave 2.4 g of a dark orange oil (component A) and 1.44 g of a dark red oil (component B). Flash chromatography of Component A (SiO2, Hexanes) and Component B (SiO2, Hexanes) separately yielded 3.2 g, 72%, of the title compound as a light peach oil. MS (+ESI): m/z 345 ([M+H]+). Step 1: 1-((4-(Difluoromethoxy)phenyl)ethynyl)-3-methylbenzene To a solution of 4-iodo(difluoromethoxy)benzene (4.64 g, 17.2 mmol) in DMF (26 mL) was added TEA (9.57 g, 13.2 mL, 94.6 mmol), PdCl2(PPh3)2 (603 mg, 0.86 mmol), CuI (98 mg, 0.516 mmol), and 3-ethynyltoluene (2.5 g, 2.78 mL, 0.90 mmol). The reaction mixture was stirred for 4 h then it was poured into water and diluted with EtOAc. The aqueous layer was separated and extracted twice more with EtOAc. The combined organic layers were dried over Na2SO4, filtered, and concentrated onto 20 g Celite. Flash chromatography (SiO2, Hexanes) gave 1.44 g of a dark red oil and 2.44 g of a dark orange oil. Both fractions were rechromatographed, separately, to provide 3.2 g, 72%, of the title compound as a light peach oil. 1H NMR 500 MHz (CDCl3) delta 2.33 (s, 3H); 6.50 (t, J=73.6 Hz, 1H); 7.06 (d, J=8.81 Hz, 2H); 7.12 (d, J=6.83 Hz, 1H); 7.20 (d, J=7.53 Hz, 1H); 7.30 (d, J=7.76 Hz, 1H); 7.33 (s, 1H); 7.47-7.51 (m, 2H)

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-(Difluoromethoxy)-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WYETH; US2009/48320; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature 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.

0.3 mmol of sodium carbonate, 0.1 mmol of 1,2-bis(3-methoxyphenyl)acetylene, 0.005 mmol of palladium acetate, and double (2-0.005 mmol of diphenylphosphoryl phenyl)ether, 0.15 mmol of pinacol borate, 0.15 mmol of 2-isopropyliodobenzene and N,N-1 mL of methylformamide was added to a 15 mL reaction tube, nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C, and reacted for 24 hours;Cool to room temperature, dilute with ethyl acetate, wash three times with water, dry with organicNa2SO4 is dried, filtered, concentrated, thin layerChromatography purification gave 20.8 mg of the desired product in a yield of 43%. The nuclear magnetic and high resolution mass spectra of this compound are characterized as follows:

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; Huaqiao University; Cheng Guolin; Lv Weiwei; (10 pag.)CN109879899; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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.

tert-Butyllithium (9.0 mL of a 1.7 mol/l solution in n-pentane, 15.3 mmol)was added to iodomesitylene (10) (1.51 g, 6.14 mmol) in Et2O (20 mL) at ?78 °C under inertatmosphere. After 30 min, CuCN (273 mg, 3.07 mmol) was added and the suspension stirred at?60 °C for 2 h. The reaction mixture was then treated with nitrobenzene (0.94 mL, 9.12 mmol)and allowed to warm up to room temperature overnight. An aqueous solution of NH3 (12.5percentw/w, 80 mL) was slowly added and the resulting residue was extracted with MTBE (3 x 50 mL).The combined organic layers were washed with water (50 mL) and brine (50 mL), dried overMgSO4, filtered, and the solvent was removed in vacuum. The product 11 could be obtained aftercolumn chromatography (SiO2, n-hexane, Rf 0.43) as a colorless solid (542 mg, 2.27 mmol,74percent), mp 98 °C (ref.27 99?100 °C). 1H NMR (300 MHz, CDCl3): delta 6.94 (s, 4 H), 2.34 (s, 6 H),1.87 (s, 12 H) ppm. 13C{1H} NMR (75 MHz, CDCl3): delta 137.0 (2 C), 136.0 (2 C), 135.5 (4 C),128.2 (4 CH), 21.1 (2 CH3), 19.8 (4 CH3) ppm. IR (ATR): 2997 (w), 2938 (m), 2916 (m), 1470(m), 1436 (m), 1375 (m), 1004 (m), 852 (s), 595 (m) cm?1. MS (EI, 70 eV), m/z (percent): 238 (99)[M+], 223 (100), 208 (33), 193 (25). Anal. calcd. for C18H22 (238.37): C 90.70, H 9.30; found C90.73, H 9.34.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Behler, Florian; Wickleder, Mathias S.; Christoffers, Jens; ARKIVOC; vol. 2015; 2; (2014); p. 64 – 75;,
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. 620-05-3, name is (Iodomethyl)benzene, A new synthetic method of this compound is introduced below., Recommanded Product: 620-05-3

General procedure: In a flame-dried round-bottom flask, beta-amidoester (9) (1 mmol; 1 equiv) was taken in DMF (5 mL) at room temperature. To this reaction mixture KOt-Bu (1.2 mmol; 1.2 equiv) was added. After 5 minutes of stirring at same temperature alkyl halide (1.05 mmol; 1.05 equiv) was added and stirring was continued for 15 minutes. Upon completion of the alkylation (judged by TLC), it was diluted with 10 mL of EtOAc and quenched with water. The organic extracts were dried over anhydrous sodium sulphate and concentrated under vacuum. The crude product was purified by flash chromatography (hexane and EtOAc as eluents) to afford compounds 10.

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; Kumar, Nivesh; Ghosh, Santanu; Bhunia, Subhajit; Bisai, Alakesh; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 1153 – 1169;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, 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 401-81-0, Safety of 1-Iodo-3-(trifluoromethyl)benzene

Dioxane (100 mL) was purged with nitrogen gas for 10 min. Phenanthrolene ( 1.0 g) and copper (I) iodide (1.0 g) were added to the dioxane, the suspension was allowed to stir under a nitrogen atmosphere for 5 min, and then cesium carbonate ( 18.72 g, 57.45 mmol), dimethyl malonate (5.46 g, 50.6 mmol), and l-iodo-3-(trifluoromethyl)benzene (12.5 g, 46.0 mmol) were added. The reaction mixture was heated to reflux for 18 h and then cooled to room temperature. Aqueous 1 N HC1 was added to the reaction mixture, the layers were separated, and the aqueous layer was extracted with ethyl acetate (3 x 100 mL). The combined organic layers were dried over magnesium sulfate and filtered. Celite diatomaceous filter aid (5 g) was added to the filtrate, and the resulting suspension was concentrated under reduced pressure at 50 C to yield a solid consisting of the crude product adsorbed onto Celite. This solid was purified by silica gel chromatography eluting with a gradient of 100% hexanes to 25% ethyl acetate in hexanes to yield 7.36 g (58.0%) of the title product. NMR (CDC13) delta 7.59-7.65 (m, 3H), 7.49 (t, 1H), 4.70 (s, 1H), 3.76 (s, 6H).

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

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; ZHANG, Wenming; ANNIS, Gary David; WO2013/90547; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

68507-19-7, name is 3-Iodo-4-methoxybenzoic 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

3-iodo-4-methoxybenzoic acid (1.00 g, 7.19 mmol) was dissolved in SOCl2 (12.0 mL) and stirred at 80 C (22 h). Next, SOCl2 was removed in vacuo and azeotroped twice with benzene to give 57 (0.700 g, 2.36 mmol, 32%) as a white solid. 1H-NMR (400 MHz) CDC13: 8.50 (s, 1 H), 8.12-8.10 (d, 1 H), 6.88-6.86 (d, 1 H), 3.99 (s, 3 H); ,3C-NMR (100 MHz) CDC13: 165.1, 162.8, 141.9, 133.2, 126.3, 109.4, 85.2, 56.2.

The synthetic route of 68507-19-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; J-PHARMA CO., LTD.; WEMPE, Michael, F.; ENDOU, Hitoshi; WO2012/48058; (2012); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com