Category: iodides-buliding-blocks

Synthetic Route of 34270-90-1,Some common heterocyclic compound, 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, molecular formula is C4H8I2O, 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.

Spiro[4H-pyran-4,9′(4’H)-pyrimido[2,1-c][1,4]thiazine]-2′-carboxylic acid, 2,3,5,6,6′,7′-hexahydro-3′-hydroxy-4′-oxo-, ethyl ester, 8′,8′-dioxide: To a stirred yellow mixture of intermediate 12 (0.189 g, 0.50 mmol) intermediate 18 (0.208 g, 0.62 mmol) in DMF (5 mL) wad added Cs2CO3 (0.332 g, 1.02 mmol) at once at room temperature. After 24 h, the reaction mixture was diluted with Et2O (50 mL), washed with water (2×10 mL), brine (10 mL), dried (Na2SO4), filtered and concentrated to give colorless paste which was used in the subsequent step without purification.

The synthetic route of 34270-90-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/112190; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 51560-21-5, The chemical industry reduces the impact on the environment during synthesis 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene, I believe this compound will play a more active role in future production and life.

Compound 8 (1.0 g, 2.56 × 10 -3 mol) was dissolved in dichloromethane (20 mL) and stirred in an ice-salt bath for 30 minutes.A 1.0 M solution of BBr3 in dichloromethane (6.14 mL, 6.14 × 10 -3 mol) was added to the solution, and the mixture was stirred overnight.afterwards,After adding deionized water to the reaction mixture until no white smoke is generated,Suction filtration was performed.The obtained solid is dried under vacuum,Compound 9 was obtained as a white solid (yield 0.81 g, 87.1%).

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, 1,4-Diiodo-2,5-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tokyo Denki University; Adachi, Naoya; Nagahori, Tomomi; (27 pag.)JP2020/2024; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 19230-28-5, These common heterocyclic compound, 19230-28-5, name is 1,3-Dichloro-2-iodobenzene, 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 toluene 3.0mL solution of tert-butyl 2-amino-4-phenethylbenzoate 0.10g were added 1,3-dichloro-2-iodobenzene 0.23g, cesium carbonate 0.22g, tris(dibenzylideneacetone)dipalladium(0) 3.0mg and 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl 8.0mg at room temperature, and it was stirred at 110C for 24 hours. After the reaction mixture was cooled to room temperature, palladium acetate 1.5mg, tris(dibenzylideneacetone)dipalladium(0) 3.0mg and 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl 8.0mg were added, and it was stirred at 110C for 20 hours. After the reaction mixture was cooled to room temperature, insoluble matter was filtrated, ethyl acetate and 10% citric acid aqueous solution were added to it. The organic layer was separated and collected, dried over anhydrous magnesium sulfate after washing with saturated sodium chloride aqueous solution, and the solvent was removed under reduced pressure. The obtained residue was refined by silica gel column chromatography [Trikonex company, Flash Tube 2008, eluent; hexane:ethyl acetate=4:1] to give tert-butyl 2-(2,6-dichloroanilino)-4-phenethylbenzoate. Trifluoroacetic acid 10mL was added to the obtained tert-butyl 2-(2,6-dichloroanilino)-4-phenethylbenzoate, and it was stirred at room temperature for 2 hours. The solvent was removed under reduced pressure, and the obtained residue was refined by reversed-phase silica gel column chromatography [eluent; 75-100% acetonitrile/0.1% trifluoroacetic acid aqueous solution] to give 2-(2,6-dichloroanilino)-4-phenethylbenzoic acid 9.4mg of white solid. 1H-NMR(DMSO-d6) delta value: 2.76(4H,m),6.04(1H,d,J=1.2Hz),6.66(1H,dd,J=8.1,1.2Hz),7 .08-7.24(5H,m),7.36(1H,t,J=8.2Hz),7.61(2H,d,J=8.3Hz),7.80(1 H,d,J=8.0Hz),9.52(1H,s),13.00(1H,s).

The synthetic route of 19230-28-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TOYAMA CHEMICAL CO., LTD.; EP1860098; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 461-17-6,Some common heterocyclic compound, 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane, molecular formula is C4H6F3I, 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.

Reference Example 69 fluoro-4-(4,4,4-trifluorobutoxy)benzoic acid By operating in the same manner as in Reference Example 68 and using 1,1,1-trifluoro-4-iodobutane, the title compound was obtained as colorless powder.1H-NMR (DMSO-d6) delta: 1.97 (2H, m), 2. 44 (2H, m), 4.13 (2H, t, J=6.3Hz), 6.89 (1H, t, J=2.0Hz), 6.90 (1H, m) 7.84 (1H, t, J=9.0Hz), 14.44 (1H, s).

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

Reference:
Patent; Takeda Chemical Industries, Ltd.; EP1447402; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 3718-88-5, name is 3-Iodobenzylamine hydrochloride, 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 3718-88-5, Recommanded Product: 3718-88-5

1.5 mL of ethanol were added to 80 mg (0.17 mmol) of benzoic acid (3aS,4R,6S,6aR)-6-(2,6-dichloropurin-9-yl)-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxol-4-yl methyl ester, 60 mg (0.22 mmol) of 3-iodobenzylamine hydrochloride, and 0.07 mL (0.49 mmol) of triethylamine, which was stirred at ambient temperature for 3 days. The reaction mixture was distilled under reduced pressure, and the concentrate was purified by silica gel column chromatography using the eluant (hexane:ethyl acetate=1:1) to obtain 102 mg (yield: 90%) of benzoic acid (3aS,4R,6S,6aR)-6-(2-chloro-6-(3-iodobenzylamino)purin-9-yl)-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxol-4-yl methyl ester as white foam. 1H-NMR(CDCl3) delta: 1.23 (s, 3H), 1.28 (s, 3H), 3.89 (t, 1H), 3.94 (dd, 1H), 4.08 (dd, 1H), 4.65 (d, 2H), 5.01 (m, 2H), 5.81 (d, 1H), 6.91-7.75 (m, 9H), 8.83 (s. 1H) UV (methanol): lambdamax 282 nm (pH 7).

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; Government of the United States of America, repres ented by The Secretary, Department of Health and; Ewha Womans University; US2005/256143; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 202865-85-8, 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. 202865-85-8, name is 1-Bromo-4-iodo-2-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

1-bromo-4-iodo-2-methylbenzene (12.5 g) and tert-butyl 5-hydroxy-4-methyl-2,3-dihydro-1H-indole-1-carboxylate (7.00 g) in dioxane (250 mL) solution, copper iodide (I) (107mg), N,N-dimethylglycine (116 mg) and cesium carbonate (18.3 g) was added, stirred for 5 hours and 30 minutes at 100C. Allowed to stand overnight, After cooling to room temperature, and stirred for 9 hours at again 100C, the reaction solution was filtered through Celite. The obtained filtrate was concentrated under reduced pressure, the residue was purified by silica gel column chromatography (dichloromethane/hexane) to give the title compound (5.26 g) as a colorless solid.

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

Reference:
Patent; DAIICHI SANKYO COMPANY LIMITED; NAGAMOCHI, MASATOSHI; GOTANDA, KENTOKU; NOGUCHI, TETSUJI; GOTO, TAIJI; SASAKI, JUNKO; TORIHATA, MUNEFUMI; YOSHINO, TOSHIHARU; ISOBE, TAKASHI; (97 pag.)JP2016/108257; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 387-48-4,Some common heterocyclic compound, 387-48-4, name is 3-Fluoro-2-iodobenzoic acid, molecular formula is C7H4FIO2, 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-fluoro-2-iodobenzoic acid (1 .4 g, 5.26 mmol), 1 H-pyrazole (0.72 g, 10.5 mmol), trans-N, N’-dimethyl-cyclohexane-1 ,2-diamine (0.17 mL, 1 .05 mmol), Cul (50.1 mg, 0.26 mmol), dioxane (50 mL) and water (0.028 mL) was added CS2CO3 (3.43 g, 10.5 mmol). The reaction mixture was heated to 100 C for 1 h. The reaction mixture was cooled to ambient temperature then diluted with water. The aqueous layer was acidified to pH2 and extracted with EtOAc (30 mL) three times. The organic layers were combined, dried over Na2SO4, filtered and concentrated. Purification (FCC), (DCM to 10%MeOH/1 %HOAC/DCM) afforded the title compound as a colorless oil (790 mg, 72%). 1H NMR (400 MHz, CDCI3): 7.85 – 7.73 (m, 1 H), 7.54 – 7.44 (m, 1 H), 7.44 – 7.34 (m, 1 H), 6.55 (s, 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Fluoro-2-iodobenzoic acid, its application will become more common.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.; WO2011/50200; (2011); 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. 624-75-9, name is 2-Iodoacetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C2H2IN

The compound obtained in Example 64 (4.6 g, 15.35 mmol) and potassium carbonate (10.6 g, 76.73 mmol) were added to acetone (100 mL) and refluxed for 2 hours. To this reaction mixture was dropwise added iodoacetonitrile (1.34 mL, 18.42 mmol), and refluxed over 2 hours. The acetone was removed by vacuum distillation, and the residue was treated in water (200 mL) and ethyl acetate (200 mL). The organic layer was dried over anhydrous magnesium sulfate and distillated in a vacuum. The concentrate was subjected to column chromatography (silica gel, ethyl acetate-hexane 2:3 v/v) to afford a mixture of 2:1 of regioisomers as yellow oil. These two regioisomers (4.16 g, 80%) were used in the next reaction step without separation.Example 65-2Preparation of 4-(2-chloropyridin-5-yl)-5-(3-methoxy-5-methylphenyl)-pyrazol-1-yl)acetonitrile1H NMR (CDCl3) delta 2.28 (s, 3H), 3.66 (s, 3H), 5.16 (s, 2H), 6.71 (s, 2H), 6.84 (s, 1H), 7.24 (d, J=8.3 Hz, 1H), 7.49 (dd, J=2.3, 5.9 Hz, 1H), 7.70 (s, 1H, 8.32 (s, 1H); 13C NMR (CDCl3) delta 21.57, 39.89, 55.23, 110.80, 113.76, 115.28, 117.76, 121.47, 124.02, 127.24, 129.92, 132.57, 138.58, 140.12, 148.71, 149.92, 151.17, 159.69, 162.33.To a solvent mixture of THF and water (4:1, 10 mL) were added the mixture prepared in Example 65 (320 mg, 0.95 mmol), 3-acetylphenylboronic acid (0.19 g, 1.13 mmol), dichlorobis(triphenylphosphine)palladium (II) (33 mg, 0.04 mmol) and potassium carbonate (0.13 g, 0.95 mmol). The reaction system was purged with nitrogen gas for 10 min, and stirred at 70 C. for 12 hours under nitrogen atmosphere. The reaction mixture was cooled at room temperature, washed with ice water (100 mL) and extracted with ethyl acetate (100 mL×3). The organic extract was dried over anhydrous magnesium sulfate and distilled under vacuum. The residue was subjected to prep-TLC using a solvent mixture of ethyl acetate/hexane to purify the desired products.Purification yield by prep-TLC (silica gel, ethyl acetate-hexane, 1:2, v/v): (202 mg); m.p. 73-74 C.; 1H NMR (CDCl3) delta 2.27 (s, 3H), 2.65 (s, 3H), 3.66 (s, 3H), 5.16 (s, 2H), 6.71 (s, 1H), 6.77 (s, 1H), 6.91 (s, 1H), 7.54 (t, J=7.7 Hz, 1H), 7.60-7.72 (m, 3H), 8.97 (d, J=7.5 Hz, 1H), 8.19 (d, J=7.5 Hz, 1H), 8.58 (s, 1H), 8.63 (s, 1H); 13C NMR (CDCl3) delta 21.55, 26.83, 39.84, 55.19, 110.91, 113.92, 115.23, 118.77, 120.03, 121.58, 126.53, 127.18, 128.77, 129.14, 129.93, 131.22, 133.02, 136.57, 137.63, 139.31, 139.97, 149.01, 151.22, 154.56, 159.68, 198.12.

The synthetic route of 624-75-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LEE, So Ha; Yoo, Kyung Ho; Oh, Chang Hyun; Han, Dong Keun; El-Deeb, Ibrahim Mustafa; Park, Byung Sun; Jung, Su Jin; US2011/15395; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 627-31-6, The chemical industry reduces the impact on the environment during synthesis 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), I believe this compound will play a more active role in future production and life.

Compound 46; 5-{N-ethyl-N-[4-[1-(3-methyl-1-(2-(1-piperidinyl)phenyl)butyl)aminocarbonylmethyl]phenyl]amino}-2,2-dimethylpentanoic acid; This product was synthesized in 3 steps: Step 1; Methyl 5-iodo-2,2-dimethylpentanoate; Under anhydrous atmosphere, diisopropylamine (2.75 ml; 19.6 mmol) in THF (5 ml) was cooled to 0 C. nButyllithium (2M in pentane, 9.8 ml; 19.6 mmol) was added dropwise. The mixture was stirred 30 min at 0 C. and cooled to -78 C. with dry ice. Methyl 2-methylpropanoate (1.0 g; 9.8 mmol) was added and the mixture was stirred for 45 min at -78 C. 1,3-diiodopropane (5.9 ml; 39.2 mmol) was added and stirring was maintained for 1 h. The mixture was slowly warmed to room temperature. The crude was neutralized upon addition of 2M HCl (25 ml) and the expected product was extracted by ethyl acetate (3×25 ml). Organic layers were combined, dried with magnesium sulfate (MgSO4), and concentrated under reduced pressure. The expected product was purified by silica gel chromatography (cyclohexane/ethyl acetate 95/5). Yield: 47%

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-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GENFIT; US2006/79696; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 204257-72-7, name is Methyl 2-fluoro-4-iodobenzoate, 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 204257-72-7, Recommanded Product: Methyl 2-fluoro-4-iodobenzoate

b. Methyl 2-fluoro-4-iodo-5-nitrobenzoate (3). A modified procedure of Kakuta and coworkers was followed.2 To a solution of methyl 2-fluoro-4-iodobenzoate (2) (1.4 g, 5.0 mmol) dissolved in concentrated sulfuric acid (5 mL) was added a solution of concentrated nitric acid (6.0 mL) and concentrated sulfuric acid (9.0 mL) dropwise at 0 C with stirring. The reaction solution was then stirred at room temperature for 5 h. The reaction solution was poured onto ice (100 mE) and extracted with ethyl acetate. The combined organic layers were washed with saturated NaHCO3 (100 mE) and brine (50 mE) and then dried over sodium sulfate, filtered and concentrated in vacuo. The crude product was purified by column chromatography (150 mL Si02, 2% ethyl acetate:hexanes to 10% ethyl acetate:hexanes) to give 3 (1.27 g, 78%) as a green crystalline solid, m.p. 84-87 C: ?HNMR (400 MHz, CDC13) oe 8.50 (d, Jz 6.4, 1H), 7.87 (d, J= 9.6, 111), 3.97 (s, 3H); ?3C NMR (100.6MHz, CDC13)6 163.1, 162.3, 162.2, 160.4, 148.7, 131.1, 130.8, 129.1, 129.0, 119.4, 119.2, 92.7,92.6, 53.1 ; JR (neat) n 2987, 1703, 1602, 1560, 1532, 1440 cm?; LC-FAB-MS (M)+ calcd forC8H5FINO4 324.9247, found 324.9249.

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-fluoro-4-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY; WAGNER, Carl; MARSHALL, Pamela; JURUTKA, Peter; WO2015/130973; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com