Tag: M.W=300-400

Related Products of 98-61-3, 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.

A solution of (2-methylpropyl)amine (121 mg,1.65mmol) and triethylamine (0.35ml, 2.47mmol) in DCM (10ml) was treated with 4-iodobenzenesulfonyl chloride (500mg,1.65mmol) by dropwise addition over 10 minutes with stirring under argon.The reaction mixture was stirred at room temperature for 16 hr. Then the reaction mixture was washed with water (10ml), separated the organic layer, dried with sodium sulphate.Solvent was removed by rotary evaporation to give the title compound as a white solid (517mg, 92%).LC/Mass Spec (ES): Found 340 (ES+), retention time 3.14mins. C10H14INO2S requires339. 1H-NMR (400MHz, CDCI3): 0.88 (6H, m), 1.72 (1 H, m), 2.78 (2H, m), 4.41 (1 H, m)7.56 (2H, m), 7.88 (2H, m).

The synthetic route of 98-61-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/107539; (2007); A1;,
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Electric Literature of 199786-58-8, These common heterocyclic compound, 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, 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.

Example 15C 5-Bromo-2-iodobenzaldehyde A solution of oxalyl chloride (1.53 g, 0.012 mol) in CH2Cl2 (15 mL) was cooled to -70 C., and DMSO (1.41 g, 0.018 mol) in CH2Cl2 (15 mL) was added at -65 to -70 C. The mixture was stirred under nitrogen for 10 minutes at -70 C. and then treated with the product from Example 15B (2.35 g, 7.5 mmol) in 60 mL CH2Cl2. The slurry was stirred at -65 C. for 15 minutes and treated with triethylamine (3.8 g, 0.037 mol). The mixture was allowed to warm to -10 C. over 1 hour. The mixture was treated with 20 mL of water and allowed to warm to room temperature. The organic layer was separated and concentrated to provide the title compound. 1H NMR (CDCl3, 400 MHz) delta 9.97. (s, 1H), 7.97 (d, J=4 Hz, 1H), 7.79 (d, J=8 Hz, 1H), 7.40 (dd, J=4, 8 Hz, 1H). MS (DCl/NH3) [M+NH4]+ at 328.

The synthetic route of 199786-58-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Altenbach, Robert J.; Black, Lawrence A.; Chang, Sou-Jen; Cowart, Marlon D.; Faghih, Ramin; Gfesser, Gregory A.; Ku, Yi-Yin; Liu, Huaqing; Lukin, Kirill A.; Nersesian, Diana L.; Pu, Yu-ming; Curtis, Michael P.; US2005/272736; (2005); A1;,
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Reference of 31827-94-8, The chemical industry reduces the impact on the environment during synthesis 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, I believe this compound will play a more active role in future production and life.

To a solution of 4-iodoacetophcnonc 4.9 ( 1 O g, 40.6 mmol) in dioxanc ( 100 mL) was added bromine (2.18 mL, 42.7 mmol) dropwise at 0 C. The reaction mixture was stirred for 30 minutes. The resulting solution was concentrated. The residue was dissolved in dichloromethane (200 mL) and was washed with satd. NaHCO3, H2O and brine, dried over Na2SO4, and concentrated to give 4.10. To a solution of 4.10 in DMF ( 100 mL) were added potassium carbonate ( 16.8 g, 122 rnmol) and /ert-butylcarbamidine hydrochloride 4.11 ( 1 1.1 g, 81.2 mmol). After stirring overnight, the reaction mixture was filtered and the filtrate was concentrated. The resulting residue was purified on silica gel using a mixture of hexanes and ethyl acetate to give 4.12 (8.1 g, 61%). LRMS (M+Na+) m/z 327.0.

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-Bromo-1-(4-iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CYTOKINETICS, INC.; SMITHKLINE BEECHAM CORPORATION; WO2007/56143; (2007); A2;,
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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C7H6BrIO

Step 1: An oven-dried flask equipped with a magnetic stir bar was charged with l-bromo-4- chloro-2-fluoro-5-methoxy-benzene (100 mg, 0.42 mmol), (4-methoxyphenyl)boronic acid (69.8 mg, 0.46 mmol) and [l,l’-bis(diphenylphosphino)ferrocene] dichloropalladium(II) complex with dichloromethane (17.1 mg, 0.021 mmol). The flask was sealed with a rubber septum, and then evacuated and backfilled with argon (repeated a total of 3 X). l,4-Dioxane (1.0 mL) and aqueous 1 M K2CO3 (0.5 mL, 0.5 mmol) were added and the reaction was heated to 90 C for 2 h. The reaction was cooled to room temperature, diluted with water (5 mL), and extracted with EtOAc (3 X). The combined organic phases were dried over Na2S04, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with a EtOAc/hexanes gradient (0-10% EtOAc) to yield l-chloro-5-fluoro-2-methoxy-4-(4- methoxyphenyl)benzene (89.2 mg, 80%) as an off white solid. (1337) MS m/z 267.8 [M+H]+; 1H NMR (CDCL) d: 7.39 (dd, /= 8.8, 1.6 Hz, 2H), 7.13 (d, /= 9.5 Hz, 1H), 6.92 (d, J= 8.8 Hz, 2H), 6.85 (d, J= 6.9 Hz, 1H), 3.85 (s, 3H), 3.79 (s, 3H).

The synthetic route of 755027-18-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PTC THERAPEUTICS, INC.; SYDORENKO, Nadiya; ALAM, Md Rauful; ARNOLD, Michael A.; BABU, Suresh; BHATTACHARYYA, Anuradha; CHEN, Guangming; GERASYUTO, Aleksey I.; KARP, Gary Mitchell; KASSICK, Andrew J.; MAZZOTTI, Anthony R.; MOON, Young-Choon; NARASIMHAN, Jana; PATEL, Jigar; TURPOFF, Anthony; WOLL, Matthew G.; YAN, Wuming; ZHANG, Nanjing; (0 pag.)WO2020/5873; (2020); A1;,
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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. 148836-41-3, name is 1-Bromo-4-chloro-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 148836-41-3

A solution of cyclopropylboronic acid (2.104 g, 24.49 mmol), 1-bromo-4-chloro-2-iodobenzene (5.700 g, 17.96 mmol), potassium phosphate (13.86 g, 65.3 mmol), and PdCl2(dppf)-DCM adduct (0.667 g, 0.816 mmol) in 18 mL dioxane and 6 mL water was heated to 100 C. overnight. The reaction mixture was then diluted with DCM and washed with water. The organics were dried over MgSO4 and concentrated. The crude residue was used in the next step without purification. m/z (ESI) does not ionize in H+ mode.

The synthetic route of 148836-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Amgen Inc.; Weiss, Matthew; Boezio, Alessandro; Boezio, Christiane; Butler, John R.; Chu-Moyer, Margaret Yuhua; Dimauro, Erin F.; Dineen, Thomas; Graceffa, Russell; Guzman-Perez, Angel; Huang, Hongbing; Kreiman, Charles; La, Daniel; Marx, Isaac E.; Milgrim, Benjamin Charles; Nguyen, Hanh Nho; Peterson, Emily; Romero, Karina; Sparling, Brian; US9212182; (2015); B2;,
Iodide – Wikipedia,
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Electric Literature of 181765-86-6,Some common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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 compound 10 (5.2 g, 0.015 mol) in dry CH2Cl2 (30 mL) was added DIBAL (30.5 mL, 1 M in THF, 30.5 mmol) at 0 C; The mixture was slowly warmed up to rt and stirred overnight. The mixture was then cooled to 0 C and quenched with citric acid (aq. 15%) slowly. The resulting mixture was extracted with CH2Cl2. The organic layer was washed with brine and dried with MgSO4. After removal of CH2Cl2 under vacuum, the resulting crude product was purified by silica column flash chromatography (hexanes/CH2Cl2, 1:1) to give compound 11 as a white solid (4.79 g, 0.0153 mol, 100%).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhou, Ningzhang; Wang, Li; Thompson, David W.; Zhao, Yuming; Tetrahedron; vol. 67; 1; (2011); p. 125 – 143;,
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. 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, A new synthetic method of this compound is introduced below., Recommanded Product: 34270-90-1

Step D: 4-(4-(2-((2,6-difluorobenzyl)oxy)-l , 1 ,1 ,3,3,3-hexafluoropropan-2-yl)phenyl)-4- ((4-fluorophenyl)sulfonyl)tetrahydro-2H-pyran Sodium hydride (13.27 mg, 0.332 mmol, 60%> suspension in mineral oil) was added to a solution of l,3-difluoro-2-(((l,l,l,3,3,3-hexafluoro-2-(4-(((4- fluorophenyl)sulfonyl)methyl)phenyl)propan-2-yl)oxy)methyl)benzene (18 mg, 0.033 mmol) and l-iodo-2-(2-iodoethoxy)ethane (32.4 mg, 0.100 mmol) in N,N- dimethylformamide (1 mL). After 1 h at room temperature, the reaction was complete as judged by LCMS analysis. The mixture was quenched with saturated ammonium chloride (1 mL), diluted with ethyl acetate (20 mL), washed with water (2×5 mL), brine (5 mL), dried (magnesium sulfate), filtered and concentrated under reduced pressure. Silica gel chromatography, eluting with 5-40% ethyl acetate in hexanes, gave Example 1 as white solid (17.4 mg, 81% yield). LC/MS (M+18): 630.1 ; LC retention time: 4.541 min (analytical HPLC Method A); 1H NMR (400 MHz, CDC13) delta ppm 7.63 (d, J=8.4 Hz, 2H), 7.44 – 7.31 (m, 3H), 7.28 – 7.19 (m, 2H), 7.03 – 6.89 (m, 4H), 4.73 (s, 2H), 4.07 – 3.96 (m, J=l 1.8, 1.7 Hz, 2H), 3.37 (t, J=1 1.2 Hz, 2H), 2.77 – 2.62 (m, 2H), 2.45 (d, J=12.3 Hz, 2H).

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; DUAN, Jingwu; DHAR, T.G. Murali; JIANG, Bin; KARMAKAR, Ananta; GUPTA, Arun Kumar; LU, Zhonghui; WO2015/103510; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 51839-15-7,Some common heterocyclic compound, 51839-15-7, name is Dimethyl 5-iodoisophthalate, molecular formula is C10H9IO4, 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 mixture of dimethyl 5-iodo-benzerte-1,3-dicarboxylate (9) (320 mg, 1.00 mmol), bis(pinacolato)diborane (10) (279 mg, 1.10 mmol), potassium acetate (294 mg, 3.00 mmol), PdCl2(dppf)* (24 mg, 0.03 mmol) and dried DMF (6 mL) was stirred at 80C for 2 h. The reaction mixture was cooled to the room temperature. Then, dimethyl 5-iodo-benzene-1,3-dicarboxylate (9) (640 mg, 2.00 mmol), PdCl2(dppf) (24 mg, 0.03) and CsF (456 mg, 3.0 mmol; dissolved in 2.5 mL of water) were added. The mixture was stirred at 80C overnight and afterwards extracted for four times with diethylether (4 x 25 mL). The organic layer was dried with MgSO4 and the solvent was removed in vacuum. The crude product was purified by column chromatography (silica gel, ethylacetate/hexane, 3:7 v/v). Yield 82 %. M.p. 214-215 C. 1H-NMR (400 MHz, CDCl3): delta= 4.00 (s, 12H), 8.51 (d, 4H, J = 1.5 Hz), 8.72 (d, 2H, J = 1.5 Hz). 13C-NMR (100 MHz, CDCl3): delta= 52.5, 130.2, 131.5, 132.3, 139.9, 165.9. Rf= 0.50 (silica gel, othylacetate/hexane, 3:7 v/v). MS-EI, m/z (%): 386 (75) [M+], 355 (100), 327 (15), 194 (10). *[1,1′-bis(diphenylphoshino)ferrocene]dichloropalladium(II)].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Dimethyl 5-iodoisophthalate, its application will become more common.

Reference:
Patent; Technische Universitaet Carolo-Wilhelmina zu Braunschweig; EP1972338; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 328-73-4, 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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: n-BuLi (1.67 M solution in hexane, 1.32 mL, 2.2 mmol) was added dropwise into a solution of p-bromochlorobenzene (383 mg, 2.0 mmol) in THF (3 mL) at -78 °C for 30 min. Then, ethyl formate (1.6 mL, 20 mmol) was added to the mixture and the obtained mixture was stirred at -78 °C. After 3 h at the same temperature, I2 (1523 mg, 6 mmol), K2CO3 (1382 mg, 10 mmol) and EtOH (3 mL) were added at -78 °C and the mixture was stirred for 14 h at rt. The reaction mixture was quenched with satd aq Na2SO3 (5 mL) and was extracted with CHCl3 (3.x.20 mL). The organic layer was washed with brine and dried over Na2SO4 to provide ethyl 4-chlorobenzoate in 77percent yield. If necessary, the product was purified by short column chromatography (SiO2:hexane:EtOAc=9:1) to give pure ethyl 4-chloro-1-benzoate as a colorless oil.

The synthetic route of 1-Iodo-3,5-bis(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ushijima, Sousuke; Moriyama, Katsuhiko; Togo, Hideo; Tetrahedron; vol. 68; 24; (2012); p. 4701 – 4709;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, molecular formula is C6H3BrINO2, 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 C6H3BrINO2

(1) Take (100mmol) 4- (9,9-dimethylphosphonium) boronic acid,32.6g (100mmol) of 2-iodo-5-bromonitrobenzene,(1%) Pd (PPh3) 4,40g (300mmol) sodium carbonate,Toluene (800mL),Ethanol (200 mL) and water (200 mL),Heated to reflux, reacted for 8h, the reaction was completed;The reaction solution was extracted with ethyl acetate, and the organic phase was concentrated.A yellow solid A was obtained;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 112671-42-8, its application will become more common.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (28 pag.)CN110698458; (2020); A;,
Iodide – Wikipedia,
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