Category: iodides-buliding-blocks

Reference of 98-61-3, A common heterocyclic compound, 98-61-3, name is 4-Iodobenzenesulfonyl chloride, molecular formula is C6H4ClIO2S, 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.

General procedure: In a typical experiment, the alkene derivative (1.5 mmol), halobenzenesulfonyl chloride derivative (1 mmol), Li2CO3 (0.222 g, 3 mmol), and PdCl2(CH3CN)2 (12.9 mg, 0.05 mmol) were dissolved in 1,4-dioxane (2 mL) under an argon atmosphere. The reaction mixture was stirred at 100 C for 24 h. After evaporation of the solvent, the product was purified by silica gel column chromatography.

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

Reference:
Article; Skhiri, Aymen; Salem, Ridha Ben; Soule, Jean-Francois; Doucet, Henri; Synthesis; vol. 48; 18; (2016); p. 3097 – 3106;,
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

4-bromo-2-fluorobenzeneboronic acid (0.50 g, 2.28 mmol) was added to a single-mouth bottle.Methyl 2-fluoro-4-iodobenzoate (0.57 g, 2.06 mmol),Potassium carbonate (0.95 g, 6.87 mmol) and[1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride (84 mg, 0.11 mmol).The reaction was stirred at 100 C for 1 h and then concentrated under reduced pressure.The residue obtained was subjected to silica gel column chromatography(PE/EA(V/V)=100/1)Purified to give the title compound as a colorless oil(0.39 g, 52%).

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

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Ren Qingyun; Liu Xinchang; Huang Jianzhou; Zhang Yingjun; S ¡¤geerdeman; (267 pag.)CN109111451; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 25245-27-6, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 25245-27-6 name is 1-Iodo-3,5-dimethoxybenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: To a solution of tetrabutylammonium bromide (1.100 g, 3.33mmol), potassium acetate (0.586 g, 3.57 mmol), and palladium acetate (0.025 g, 0.11mmol) in DMF (20 mL) were added substituted iodobenzene (2.21mmol) and substituted styrene (2.44 mmol). The reaction mixture was recharged with argon and stirred at 80C for 5 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, 10:3) to afford pure product.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-3,5-dimethoxybenzene, and friends who are interested can also refer to it.

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

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. 144-48-9, name is 2-Iodoacetamide, A new synthetic method of this compound is introduced below., Recommanded Product: 144-48-9

To a solution of 4-aminomethyl-3-hydxoxy-benzonitrile hydrochloride (BB1, 2.0 g) and triethylamine (2.19 g) in dichloromethane (20 ml) was added di-tert-butyldicarbonate (2.41 g). The mixture was stirred at r.t. for 3.5 h. The mixture was washed with water (3x), dried, filtered and concentrated. The crude product was dissolved in DMF (15.5 ml). Cesium carbonate (4.00 g) and iodoacetamide (2.27 g) were added and the mixture was stirred at r.t. for 3 days. Water was added and the mixture was extracted with EtOAc. The org. phase was washed with water, dried, filtered and concentrated. The crude product was dissolved in MeOH and then concentrated to obtain a thick suspension. The solid was filtered off and washed with a small amount of MeOH. This procedure was repeated with the mother liquor to give (2-carbamoylmethoxy-4-cyano-benzyL)-carbamic acid tert-butyl ester (a total of 1.88 g) as a colorless solid. MS 304.2 ([M-HD The BOC protecting group of (2-carbamoylmethoxy-4-cyano-benzyl)-carbamic acid tert-butyl ester was removed using HC1 in dioxane to give 2-(2-aminomethyl-5-cyano-phenoxy)-acetamide hydrochloride as an off-white powder. MS 206.1 ([M+H]+)

The synthetic route of 144-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2006/27135; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 2468-56-6, 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. 2468-56-6, name is 6-Iodohex-1-yne belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of N-(2-methyl-5′-(piperazin-l-yl)-6′-((tetrahydro-2H-pyran-4- yl)oxy)-[3,3′-bipyridin]-5-yl)-3-(trifluoromethyl)benzamide (22 mg, 0.041 mmol) in DMF (0.5 mL) was added potassium carbonate (8.4 mg, 0.061 mmol) and the mixture was stirred at rt for 10 min. Then, 6-Iodo-l-hexyne (7.5 uL, 0.057 mmol) was added. The mixture was stirred at rt for 65 h, diluted with water and saturated aqueous solution of ammonium chloride. After being stirred for 5 min, the mixture was diluted with EtOAc. The phases were separated and the aqueous layer was extracted twice with EtOAc. The combined organics were washed with brine, dried over sodium sulfate, and concentrated. The residue was purified by flash chromatography on silica gel using a gradient of methanol in DCM (0-15%) to afford the title compound (16 mg, 63%) as a white solid. MR (600 MHz, CDCb) delta 8.63 (d, J = 2.0 Hz, 1H), 8.35 (s, 1H), 8.16 (s, 1H), 8.12 – 8.07 (m, 2H), 7.82 (d, J = 7.7 Hz, 1H), 7.71 (d, J = 1.4 Hz, 1H), 7.64 (t, J = 7.8 Hz, 1H), 7.03 (d, J = 1.3 Hz, 1H), 5.44 – 5.36 (m, 1H), 4.03 – 3.92 (m, 2H), 3.75 – 3.63 (m, 2H), 3.19 (s, 4H), 2.66 (s, 4H), 2.49 (s, 3H), 2.47 – 2.41 (m, 2H), 2.27 – 2.21 (m, 2H), 2.18 – 2.11 (m, 2H), 1.93 – 1.83 (m, 3H), 1.72 – 1.63 (m, 2H), 1.61 – 1.54 (m, 2H). LRMS (m/z) calculated, 621.292; found, 624.8 (M+H)+.

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, 6-Iodohex-1-yne, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; QUARTZ THERAPEUTICS, INC.; ZAMBONI, Robert; HENNING, Ryan; JI, Alan; SMITH, Tyler; HELLER, Bradley; REDDY, Thumkunta Jagadeeswar; ROCHELEAU, Sylvain; BEAULIEU, Marc Andre; (266 pag.)WO2018/200981; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 69113-59-3, name is 3-Iodobenzonitrile, 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 69113-59-3, Recommanded Product: 3-Iodobenzonitrile

One equivalent of a substituted aromatic or heteroaromatic nitrile (here a compound of formula II, wherein R1 is phenyl, R7 is I1 X is (CH2)P and p = 0) is dissolved in 1 ,4-dioxane. After addition of 1 ,3 equivalents of a straight or branched chain alcohol of formula III (wherein R9 is (CH2)q and q is 1 – 10), HCI-gas is introduced at 1O0C for 6h. The resulting pellet (compound of formula IV) is filtered, washed with dioxane and dried in vacuum. EPO IVa) 3-lodo-benzimidic acid ethyl ester hydrochloride: 6.05 g (81%), colourless powder; HPLC: 2.11 min; LC-MS: 262.0 m/z.

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, 3-Iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GMBH; WO2006/131186; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 6940-76-7, 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. 6940-76-7, name is 1-Chloro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

10.16g(50mmol) of 2-(3′,4′ -dimethoxyphenyl)-3-methylbutyronitrile was dissolved in 80ml of anhydrous toluene, and 3.90g(100mmol) of sodium amide was added in fractional amounts while being stirred. After being heated and refluxed at 120 C for 2 hours, the mixture was cooled down to 80C and, with 15.33g(75mmol) of 1-chloro-3-iodopropane added thereto, further stirred at 80 C for 1 hour. After disappearance of the starting material was checked, a small amount of methanol was added to the mixture to decompose excess sodium amide, and the solvent was evaporated out under a vacuum. The residue was extracted with ethyl acetate and then washed with water until it became neutral. The organic layer was filtrated through 1PS filter paper, and then the solvent was evaporated out. The residue was purified by silica gel column chromatography, to give 12.03g(41mmol, 81%) of 5-chloro-2-(3′,4′ -dimethoxyphenyl)-2-isopropylpentanenitrile. 1H-NMR (d, CDCl3):0.82 (3H, d, J=6.7Hz), 1.21 (3H, d, J=6.7Hz), 1.38-1.54 (1H, m), 1.80-1.98 (1H, m), 2.00-2.30 (3H, m), 3.45-3.54 (2H, m), 3.89 (3H, s), 3.90 (3H, s), 6.82-6.96 (3H, m).

The synthetic route of 1-Chloro-3-iodopropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shiseido Co., Ltd.; EP1488776; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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 1A ethyl (2E)-3-(3-iodophenyl)acrylate To a suspension of NaH (60% dispersion in mineral oil) (120 mg, 3.0 mmol) in THF (20 mL) was added triethyl phosphonoacetate (436 muL, 2.2 mmol) dropwise. 3-iodo-benzaldehyde (465 mg, 2.0 mmol) was added after the bubbling has stopped. The reaction mixture was stirred at room temperature for 15 minutes. Solid NH4Cl was added, followed by 1N HCl to quench the reaction. The mixture was taken up in ethyl acetate and water. The organic phase was washed with aqueous NaHCO3, brine, dried (MgSO4), filtered and concentrated under reduced pressure and purified by flash chromatography on silica gel with hexane/ethyl acetate (4:1) to provide the titled compound (605 mg).

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

Reference:
Patent; Xin, Zhili; Liu, Gang; Pei, Zhonghua; Szczepankiewicz, Bruce G.; Serby, Michael D.; Zhao, Hongyu; US2004/167188; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 1643-29-4, name is 3-(4-Iodophenyl)propanoic acid, 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 1643-29-4, Recommanded Product: 3-(4-Iodophenyl)propanoic acid

A suspension of 3-(4-iodophenyl)propanoic acid (19) (0.50 g,1.81 mmol), bis(pinacolato)diboron (0.69 g, 2.72 mmol), and KOAc(0.71 g, 7.24 mmol) in DMF (1 ml) was degassed by bubbling argon through the mixture for 15 min, then Pd(dppf)Cl2 (66 mg,0.09 mmol) was added to this mixture. The reaction was heated to 80 C for 2.5 h. The reaction mixture was cooled to rt, filtered through a pad of silica gel, and washed with EtOAc. The filtrate was concentrated under reduced pressure and purified by column chromatography on silica gel (EtOAc in petroleum ether, 1:2) to give the product 20 (0.32 g, 63%) as a white solid. 1H NMR(300 MHz, CDCl3) d: 10.43 (b s, 1H), 7.75 (d, J = 8.0 Hz, 2H), 7.22(d, J = 8.0 Hz, 2H), 2.98 (t, J = 7.8 Hz, 2H), 2.68 (t, J = 7.8 Hz, 2H),1.34 (s, 12H). LCMS (ESI) m/z: 277.09 [M+H]+.

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:
Article; Bobileva, Olga; Ikaunieks, Martins; Duburs, Gunars; Mandrika, Ilona; Petrovska, Ramona; Klovins, Janis; Loza, Einars; Bioorganic and Medicinal Chemistry; vol. 25; 16; (2017); p. 4314 – 4329;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 82998-57-0,Some common heterocyclic compound, 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, molecular formula is C8H7IO2, 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 19; 4-Methyl-3-(4,4,5,5-tetramethyl[1 ,3,2]dioxaborolan-2-yl)benzoic acid; To a solution of 3-iodo-4-methylbenzoic acid (3.71 g, 14.2 mmol) in DMF (130 mL), bis(pinacolato)diboron (7.20 g, 28.4 mmol), [1 ,1′-bis(diphenylphosphino) EPO ferrocene]dichloro-palladium (II) (1.04 g, 1.28 mmol) and potassium acetate (6.95 g, 70.9 mmol) were added under argon. The mixture was heated at 80 0C overnight and then allowed to cool to room temperature. The solvent was evaporated and the residue was diluted with water and EtOAc. The phases were separated and the aqueous phase was extracted with EtOAc. The combined organic phases were washed twice with 3N HCI and dried over Na2SO4. The solvent was evaporated and the crude product thus obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford the title compound impurified with starting bis(pinacolato)diboron. The product was slurried in hexane, filtered and dried under vacuum to afford 2.41 g of pure material (yield: 65%). 1H NMR (300 MHz1 CDCI3) delta (TMS): 1.36 (s, 12 H), 2.61 (s, 3 H)1 7.25 (d, J = 8.1 Hz1 1 H), 8.02 (dd, J = 8.1 Hz1 J1 = 2.1 Hz, 1 H)1 8.48 (d, J = 2.1 Hz, 1 H). LC-MS (method 1): tR = 7.57 min; m/z = 261.0 [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 3-Iodo-4-methylbenzoic acid, its application will become more common.

Reference:
Patent; J. URIACH Y COMPANIA S.A.; WO2007/339; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com