Author: Jessica.F

These common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, 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. category: iodides-buliding-blocks

14.4: (3-iodo-benzyl)-dimethyl-amineTo a cold (0C) solution of 3-iodo-benzaldehyde (3g, 12.9 mmol) in anhydrous di- chloromethane (130 ml) were added acetic acid (1 .9ml) and N,N-dimethylacetamide. The yellow solution is stirred 10 minutes at 0C and sodium triacetoxyborohydride (6.85g, 32.33 mmoles) is added by portions. The resulting mixture is stirred at room temperature for 90 minutes and evaporated to dryness under reduced pressure. Ethyl acetate and a saturated aqueous hydrogen carbonate solution were added to the residue and the two layers were separated The organic phase was washed with water, dried over anhydrous sodium sulfate, filtered and concentrated under vacuum to yield (3-iodo-benzyl)-dimethyl-amine (3.05g, 90%) as a brown oil.LC/MS (Method LC8): Rt = 0.86 min; m/z = 262 [M+H]+.

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

Reference:
Patent; SANOFI; LOEHN, Matthias; MENDEZ-PEREZ, Maria; PFEIFFER-MAREK, Stefania; KANNT, Aimo; BEGIS, Guillaume; JEANNOT, Frederic; DUCLOS, Olivier; WO2013/37390; (2013); A1;,
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Synthetic Route of 444-29-1, These common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, 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.

1.0 mmol of 2-iodotrifluoromethylbenzene,1.2 mmol sodium azide,0.15 mmol DBUAnd 0.1mmol of copper acetate were sequentially added to a reaction flask equipped with 3mL of dimethyl sulfoxide,The reaction mixture was stirred at 95 ° C for 4 h,TLC was followed until the reaction was complete,A few drops of aqueous ammonia were added to the reaction mixture,Then extracted with ethyl acetate (10 mL × 3),Then washed once with saturated saline,dry,Suction filtration,Remove the solvent,Purification by column chromatography gave the desired product,Yield 72percent.

Statistics shows that 1-Iodo-2-(trifluoromethyl)benzene is playing an increasingly important role. we look forward to future research findings about 444-29-1.

Reference:
Patent; Henan Normal University; Jiang Yuqin; Zhao Yaru; Ma Suhao; Li Xingfeng; Dong Wenpei; Xu Guiqing; (10 pag.)CN106588693; (2017); A;,
Iodide – Wikipedia,
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Synthetic Route of 63262-06-6,Some common heterocyclic compound, 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, molecular formula is C6H2Br2I2, 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.

Under an argon atmosphere, dibromodiiodobenzene (2.5 g, 5.1 mmol), Intermediate 3 (4.97 g, 15.4 mmol), and Pd(PPh3)4 (237 mg, 0.205 mmol) were dissolved in toluene (250 mE) and dimethylsulfoxide (DMSO, 50 mE), 2 MNa2CO3 aqueous solution (13 mE) was added thereto, and the mixture was stirred with heating at 90 C. for 24 hours. Afier completion of the reaction, toluene was removed under reduced pressure, and the precipitated solid was filtered off. This solid was washed with methanol and ethyl acetate,whereby obtaining a white solid (2.5 g, yield: 75%). The obtained solid was Intermediate 4, which is an intended product, and by mass spectrum analysis, it was confirmed that it had an mle value of 626 with respect to a molecular weight of 626.

The synthetic route of 63262-06-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; Takahashi, Ryota; Ikeda, Hidetsugu; Seda, Keita; Nakano, Yuki; (152 pag.)US10249832; (2019); B1;,
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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Product Details of 444-29-1

General procedure: A dried round-bottomed flask was charged with aryl iodide (0.30 mmol, 1.0 equiv), ortho-bromobenzoyl chlorides (0.36 mmol, 1.2 equiv), norbornadiene (0.60 mmol, 2.0 equiv), Pd(OAc)2 (5 mol %), triphenylphosphine (12.5 mol %), Cs2CO3 (0.675 mmol, 2.25 equiv), and DMF (4 mL). The mixture was stirred at 105 C under nitrogen atmosphere for 10 h. After cooling to room temperature, the mixture was diluted with ethyl acetate (5 mL) and brine (10 mL), and extracted with ethyl acetate (3 × 10 mL). The combined organic phase was washed with brine, dried with anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate as eluent) to afford the target compounds

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhong, Yue; Wu, Wen-Yu; Yu, Shao-Peng; Fan, Tian-Yuan; Yu, Hai-Tao; Li, Nian-Guang; Shi, Zhi-Hao; Tang, Yu-Ping; Duan, Jin-Ao; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 291 – 298;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 5876-51-7,Some common heterocyclic compound, 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, molecular formula is C7H5IO2, 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.

General procedure: To a mixture of Pd(PPh3)2Cl2(0.086g, 0.12 mmol), CuI (0.047 g, 0.24 mmol), Et3N (0.51 mL, 3.66 mmol) in MeCN (20 mL) were added substituted thienylacetylene (2.44 mmol) and3,4-methylenedioxy-iodobenzene(2.21 mmol). The reaction mixture was recharged with Argon and stirred at 80C for 3 h in a sealed tube. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl and concentrated in vacuo. The residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 10:1) to afford pure product.5-(Thiophen-3-ylethynyl)benzo[d][1,3]dioxole (72).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Iodobenzo[d][1,3]dioxole, its application will become more common.

Reference:
Article; Liang, Jian-Hua; Yang, Liang; Wu, Si; Liu, Si-Si; Cushman, Mark; Tian, Jing; Li, Nuo-Min; Yang, Qing-Hu; Zhang, He-Ao; Qiu, Yun-Jie; Xiang, Lin; Ma, Cong-Xuan; Li, Xue-Meng; Qing, Hong; European Journal of Medicinal Chemistry; vol. 136; (2017); p. 382 – 392;,
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 216393-67-8 as follows. SDS of cas: 216393-67-8

4-Chloro-2-fluoro-6-iodoaniline (2.5 g, 9.2 mmol), pyruvic acid (2.5 g, 27 mmol) and DABCO (3.1 g, 27 mmol) were dissolved in DMF (15 mL). The solution was degassed and palladium acetate (500 mg) was added. The reaction mixture was heated at 100 C for 3 h, cooled to RT and then filtered. The filtrate was diluted with EA (90 mL), washed with 2M HC1 (20 mL x 3), water (40 mL) and brine (40 mL). The organic phase was dried over MgS04, filtered and evaporated to give 5-chloro-7-fluoro-lH-indole-2-carboxylic acid (1.9 g, 97% yield) as a dark solid. 1H NMR (400 MHz, DMSO^): d 13.06 (br s, 1H), 12.50 (s, 1H), 7.59 (s, 1H), 7.21 (d, = 1.2 Hz, 1H), 7.16-7.15 (t, 7= 3.2 Hz, 1H).

According to the analysis of related databases, 216393-67-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PADFORWARD LLC; KANOUNI, Toufike; (109 pag.)WO2019/152883; (2019); A1;,
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

Application of 76801-93-9, These common heterocyclic compound, 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, 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.

compound of formula [2] 5-amino-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-1,3-phthalamideReacts with acetic anhydride,The temperature is raised to 65 C -70 C for 2-6 hours, and the TLC monitoring reaction is completed.Concentrated under reduced pressure to obtain a compound of the formula [3]5-acetamido-2,4,6-triiodo-N,N’-bis(2,3-diacetoxypropyl)-1,3-phthalic acid amide;

Statistics shows that 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide is playing an increasingly important role. we look forward to future research findings about 76801-93-9.

Reference:
Patent; Tianjin Heqing Chemical Co., Ltd.; Liu Guoping; Li Yi; (7 pag.)CN108191690; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 111771-08-5, name is 2-Fluoro-6-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. Recommanded Product: 111771-08-5

To a round-bottomed flask equipped with an overhead magnetic stirrer, reflux condenser, and nitrogen inlet were added 2-Fluoro-6-iodobenzoic acid (2.5 g, 9.4 mmol), Cul (0.09 g, 0.47 mmol), and CS2CO3 (6.1 g, 18.8 mmol). To these solids were added dioxane (12.5 ml_), water (0.05 ml_), 1 H-1 ,2,3-triazole (1.09 ml_, 18.8 mmol), and finally (1 R,2R)-N1 ,N2-dimethylcyclohexane-1 ,2-diamine (0.3 ml_, 1.88 mmol). The mixture was then warmed to 100 C ON. The day after the mixture was cooled and MTBE and water were added. After vigorous mixing, the layers were separated and the bottom aqueous layer was acidified to pH 2 with 6N HCI. The aqueous phase was then extracted with DCM (3x). The combined organic layers were dried, and concentrated The residue was purified by FC on S1O2 column (eluent : from DCM to DCM:MeOH 90:10) to afford 2-fluoro-6-(2H-1 ,2,3-triazol-2-yl)benzoic acid (p186, 1.1 g, y= 56%). MS (m/z): 208.0 [M+H]+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 111771-08-5, its application will become more common.

Reference:
Patent; CHRONOS THERAPEUTICS LIMITED; MICHELI, Fabrizio; BERTANI, Barbara; GIBSON, Karl Richard; DI FABIO, Romano; RAVEGLIA, Luca; ZANALETTI, Riccardo; CREMONESI, Susanna; POZZAN, Alfonso; SEMERARO, Teresa; TARSI, Luca; LUKER, Timothy Jon; (275 pag.)WO2019/43407; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 71838-16-9, These common heterocyclic compound, 71838-16-9, name is 2-Bromo-1-iodo-4-methylbenzene, 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 activated Zn (1.2g, 19mmol) in DMA (7mL) was added bromodifluoromethyldiethyl- phosphonate (5.0g, 19mmol) in DMA (7mL). The resulting mixture was stirred at 45C for 3 hours, after which copper(I) bromide (2.7g, 19mmol) was added and stirring was continued for 0.5 hours at room temperature. 3-Bromo-4-iodotoluene (2.8g, 9.4mmol) was then added and the mixture was sonicated at room temperature for 12 hours. The reaction mixture was partitioned between ether and H2O, filtered through Celite, and the organic layer was dried over MgSO4 and concentrated in vacuo to yield 2.1 g (63%) of 27 as a clear, colorless oil;1H NMR (300 MHz, CDCl3) delta 7.51 (d, J = 6 Hz, 1 H), 7.27 (s, 1 H), 7.20 (d, J= 7.5 Hz, 1 H), 4.27 (m, 4 H), 1.36 (t, J = 8.1 Hz)

Statistics shows that 2-Bromo-1-iodo-4-methylbenzene is playing an increasingly important role. we look forward to future research findings about 71838-16-9.

Reference:
Patent; CENGENT THERAPEUTICS, INC.; WO2006/9876; (2006); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com