Author: Jessica.F

Synthetic Route of 74-88-4, 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. 74-88-4, name is Iodomethane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of N-(tert-butoxycarbonyl)-L-isoleucine (1.24 g, 5.4 mmol, 1.0 equiv) in 35 mL THF was cooled to 0 C and slowly treated with NaH (60 % in mineral oil; 0.64 g, 16.1 mmol, 3.0 equiv). CH3I (6.1 g, 42 mmol, 8.0 equiv) was added and the reaction was stirred for 24 h at ambient temperature. Diethyl ether was added and the organic layer was washed with H2O twice. The combined aqueous layers were acidified with citric acid (pH 3) and extracted with EtOAc. The combined organic phases were washed with Na2S2O3 solution and brine and dried over Na2SO4. Removal of the volatiles left the title compound as a colourless oil (1.18 g, 90%). IR 2971 (w), 2934 (w), 2880 (w), 1741 (m), 1694 (s), 1478 (w), 1457 (m), 1436 (m), 1392 (m), 1366 (m), 1332 (m), 1312 (m), 1198 (m), 1143 (s), 1047 (w), 1033 (w), 999 (m), 937 (w), 913 (w), 868 (w), 772 (m), 727 (w). 1H NMR (500 MHz, CDCl3) delta 0.90 (t, J = 7.4 Hz, 3H, H-6), 0.99 (d, J = 6.6 Hz, 3H, H-4), 1.10 (ddd, J = 13.7, 8.9, 7.4 Hz, 1H, H-5a), 1.47 (br s, 10H, H-10/11/12 & H-5b, overlapped), 1.94-2.14 (m, 1H, H-3), 2.86 (s, 3H, H-7), 4.26 (m, 1H, H-2), 9.46 (br s, OH). 13C NMR (125 MHz, (CD3)2SO) delta 10.3 (C-6), 15.8 & 15.9 (C-4), 24.6 (C-5), 27.9 (C-10/11/12), 30.3 & 30.7 (C-7), 32.8 & 33.0 (C-3), 61.4 & 63.0 (C-2), 79.1 (C-9), 154.8 & 155.3 (C-8), 172.1 (C-1). HRMS (ESI) m/z [M-H]- calcd for C12H22NO4- 244.15433, found 244.15495. [alpha]20D +2.6 (c 1.8, CH3CO2H).

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

Reference:
Article; Wunder, Anja; Rothemund, Matthias; Schobert, Rainer; Tetrahedron; vol. 74; 38; (2018); p. 5138 – 5142;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 460-37-7, 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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Fluorene (6.64 g, 40 mmol) was dissolved in 27 mL of THF. After replacing the atmosphere in a reaction vessel with a nitrogen gas, the solution thus obtained was cooled to -20 C. After adding dropwise 15.8 g of n-butyllithium (1.6 M hexane solution) in a reaction vessel, the temperature of the reaction solution was returned to room temperature. Then, the reaction solution was stirred for one hour. The reaction solution was cooled to -78 C. and 8.96 g (80 mmol) of 1-iodo-3,3,3-trifluoropropane was gradually added. The mixture thus obtained was reacted by stirring for one hour after heating to room temperature. After the reaction, 90% acetic acid was added to the mixture, and then a saturated saline solution and hexane were added. The mixed solution thus obtained was separated into the organic layer and the aqueous layer. After the organic layer thus obtained was dehydrated over anhydrous sodium sulfate, the solvent was removed from the organic layer using a rotary evaporator to obtain 6.45 g (yield: 45%) of 9,9-di-3,3,3-trifluoro-n-propylfluorene.

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, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TOKYO OHKA KOGYO CO., LTD.; TADOKORO, Yoshinori; SHIOTA, Dai; (43 pag.)US2017/160636; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

29289-13-2, name is 2-Iodo-4-methylaniline, 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. HPLC of Formula: C7H8IN

As shown in Fig. 24A, to a solution of 2-iodo-4-methylaniline (10 g, 0.0429 mol) in tetrahydrofnran (200 mL) at 0C was added NaHMDS (94.42 mL, 1 M in THF, 0.0944 mol) slowly while maintaining the internal temperature below 5C over 30 min.. After 30 min stirring at 0C, a solution of BOC anhydride (10.29 g, 0.0472 mol) in THF (50 mL) was slowly added while maintaining the internal temperature below 5 C over 30 min. The reaction mixture was warmed to room temperature and stirred 1 hr. Saturated NH4C1 (200 mL) was added to quench the reaction. The organic layer was separated and washed with water (200 mL). The combined aqueous layer was extracted with ethyl acetate (2 x 150 mL), the layers were separated. The ethyl acetate layer was combined with the organic layer and concentrated in vacuo to give brown oil. The crude compound was purified by column chromatography (0-5% ethyl acetate/hexanes). Compound 10 was obtained as a light yellow liquid (13.1 g, 91%).

The synthetic route of 29289-13-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EINZIGER, Michael; SIMPSON, Ann, Marie; (499 pag.)WO2019/200232; (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. 74-88-4, name is Iodomethane, A new synthetic method of this compound is introduced below., Safety of Iodomethane

3,4-Dimethoxy-5-iodo-benzaldehyde (compound 102, FIG. 1) A mixture of 5-iodovanillin (7 g, 25.18 mmole), potassium carbonate (8.78 g, 63.53 mmole) and iodomethane (6.43 g, 45.30 mmole) was suspended in 60 mL of DMF and stirred at room temperature for 14 hours. The reaction mixture was quenched with water and extracted with diethyl ether. The organic layer was dried over MgSO4, filtered and evaporated in vacuo to obtain a solid which was recrystallized from hexane/ethyl acetate (2:1) (6.28 g, 85.4%).

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; CytoMed, Inc.; US5358938; (1994); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 455-13-0, name is 4-Iodobenzotrifluoride, 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. Computed Properties of C7H4F3I

General procedure: A 25 mL Schlenk tube was charged with Cu2O (0.05 mmol), ArX (0.5 mmol), NHR1R2 (0.75 mmol), NaOH (1 mmol), TBAB (0.1 mmol), L2 (0.1 mmol) and H2O/EtOH (1 mL, 1/1, v/v). The mixture was stirred at 120 C for 12 h. The reaction mixture was extracted with ethyl acetate (3 10 mL), washed with water and brine, dried over anhydrous Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatograph on silica gel(ethyl acetate/petroleum ether as the eluent) to provide the target products 3a-3w and 6.

The synthetic route of 4-Iodobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Article; Xie, Jian-Wei; Yao, Zhen-Bin; Wang, Xiao-Chuang; Zhang, Jie; Tetrahedron; vol. 75; 27; (2019); p. 3788 – 3792;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 5100-98-1, name is 3-Chloro-2-iodotoluene, molecular formula is C7H6ClI, 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: 5100-98-1

To a souton of I nethybenzene (4.0 g, 16 mmo) n CC4 (12 mL), were added Nbromosuccnmde (NBS) (5.6 g, 32 nno) and 11azobs(cycohexanecarbonftre (ABN) (3.9 g, 16 mmo). Then,xture was degassed wfth nitrogen and then heated at 90 °C for I h. After coohng to rt,sHca ge was added, and the sovent was removed in vacuo. Purflcaton (FCC, SO2; 0 ? 5percent EtOAc/hexanes) provded the Ute compound as an o (3.7 g, 70percent yed). 1H NMR(400 MHz, CDC3): 3 7.37 (rn, 2H), 7.29 – 7.23 (m, I H), 4.65 (s, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5100-98-1, its application will become more common.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; RAVULA, Suchitra; SWANSON, Devin M.; SAVALL, Bradley M.; AMERIKS, Michael K.; (250 pag.)WO2016/176449; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3058-39-7, 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. 3058-39-7, name is 4-Iodobenzonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Styrene (1.4mmol) was added to a stirring mixture of arylhalide (1.0 mmol), K2CO3(1.5 mmol), nano-pd catalyst(1.5mol%), TBAB (0.5mmol) in DMF (3.0mL) and thenthe reaction mixture was heated at 130 C for the appropriatetime. The mixture was cooled down to room temperatureand the catalyst was isolated using an externalmagnet. Then, the residue was diluted with H2O(10.0mL)and extracted with EtOAc (10 × 3). The combined organicphases were combined and dried over anhydrous Na2SO4.Concentration of the mixture and column chromatographyon silica gel afforded the desired cross-coupling productsin high yield.

The synthetic route of 4-Iodobenzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Article; Khalili, Dariush; Banazadeh, Ali Reza; Etemadi-Davan, Elham; Catalysis Letters; vol. 147; 10; (2017); p. 2674 – 2687;,
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. 127654-70-0, name is 1-Chloro-3-fluoro-2-iodobenzene, A new synthetic method of this compound is introduced below., Computed Properties of C6H3ClFI

1-Chloro-3-fluoro-2-iodobenzene (100 g, 0.39 mol), (5-bromo-2-methoxyphenyl) boronic acid (90.0 g, 0.39 mol) Dissolved in 2000 mL of tetrahydrofuran. To this was added a 2M solution of sodium carbonate (Na2CO3) (750 mL) Tetrakis (triphenylphosphine) palladium (0) (4.5 g, 3.9 mmol) was added and refluxed for 9 hours. After the reaction was completed, the reaction mixture was cooled to room temperature, The water layer was separated and removed, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The mixture was recrystallized from chloroform and ethanol to give Compound A1 (104.9 g, yield 86%, MS: [M + H] + = 315 ).

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; LG Chem, Ltd.; Lee Jeong-ha; Park Tae-yun; Jeong Min-u; Lee Dong-hun; Moon Jeong-uk; (77 pag.)KR2018/41607; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

699016-40-5, name is 2-Fluoro-4-iodobenzaldehyde, 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. Safety of 2-Fluoro-4-iodobenzaldehyde

Under nitrogen at room temperature, to a solution of 2,2,2-trifluoro-N-[(1R)-2-(4-mercaptophenyl)-1-methylethyl]acetamide (4.0 g) in N,N-dimethylformamide (40 ml) was added 2-fluoro-4-iodobenzaldehyde (4.18 g) and potassium carbonate (2.31 g), and the mixture was stirred at 60 C. for 2 hours.The resulting mixture was poured into water and the aqueous mixture was extracted with ethyl acetate.The organic layer was washed successively with water (two times) and brine, dried over anhydrous magnesium sulfate and evaporated under reduced pressure.The residue was purified by column chromatography on silica gel (chloroform/ethyl acetate=10:1) to give 2,2,2-trifluoro-N-[(1R)-2-[4-[(2-formyl-5-iodophenyl)thio]phenyl]-1-methylethyl]acetamide (5.02 g). (+)ESI-MS (m/z): 516 (M+Na)+

The synthetic route of 699016-40-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FUJISAWA PHARMACEUTICAL CO., LTD.; US2004/106653; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 887266-99-1, name is 3-Fluoro-4-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 887266-99-1, COA of Formula: C7H3FIN

To a solution of 3-fluoro-4-iodobenzonitrile (2.7 g, 0.010 mmol) in DMSO (6.0 mL), K2C03 (0.450 g, 0.003 mmol) and 30% H2O2 (2.4 mL) were added at 0-10C and the reaction mass was stirred at RT for 2 h. After completion of the reaction, the reaction mass was quenched in ice cold water. The obtained solid product was filtered off to afford 2.0 g of the desired title product. 1H NMR (400 MHz, DMSO d6): delta 7.48- 7.51 (m, 2H), 7.66 (br s, 1H), 7.69- 7.70 (m, 1H), 8.09 (brs, 1H).

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-Fluoro-4-iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant Atmaram; MUTHUKAMAN, Nagarajan; KHAIRATKAR-JOSHI, Neelima; KATTIGE, Vidya Ganapati; WO2013/186692; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com