Month: June 2021

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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, A new synthetic method of this compound is introduced below., Formula: C7H6BrIO

General procedure: A solution of the disulfide 5 (1.0 equiv) in anhydrous CH2Cl2was treated with TiCl4 (3.3 equiv) and subsequently MoCl5 (3.0equiv) or with MoCl3(HFIP)2 (3.0 equiv). Subsequently, a solutionof the aromatic compound (5.0 equiv) in anhydrous CH2Cl2was added dropwise,e and the mixture was stirred for the giventime (10-60 min) at r.t. at argon atmosphere. After completionof the reaction, a sat. aq solution of NaHCO3 was added and itwas stirred for additional 5 min. The mixture was extractedwith CH2Cl2, washed with brine, dried over MgSO4, and thesolvent was evaporated. The crude product was purified asdescribed below.

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:
Article; Franzmann, Peter; Beil, Sebastian B.; Winterscheid, Peter M.; Schollmeyer, Dieter; Waldvogel, Siegfried R.; Synlett; vol. 28; 8; (2017); p. 957 – 961;,
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. 263351-43-5, name is tert-Butyl 3-iodobenzylcarbamate, A new synthetic method of this compound is introduced below., Quality Control of tert-Butyl 3-iodobenzylcarbamate

[3-(3-dimethylamino-propylamino)-benzyl]-carbamic acid tert-butyl ester; A mixture of (3-iodo-benzyl)-carbamic acid tert-butyl ester (150mg, 0.450mmol), 3 -(dimethylamino)-l -propylamine (0.084mL, 0.675mmol), K2CO3 (129mg, 0.933 mmol), CuI (1 lmg, 0.058 mmol), L-proline (13mg, 0.113mmol) and DMSO (3 mL) was heated at 8O0C for 1.5h. The reaction was cooled, poured onto water and the aqueous layer extracted with EtOAc (x3). The organic layers were combined and washed with water, brine and dried (Na2SO4). Chromatography (MeOH/EtOAc) afforded [3-(3-dimethyl amino-propylamino)-benzyl]-carbamic acid tert-buty ester (65mg) as a yellow solid, m/z (M+l) 308.13.

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; FOREST LABORATORIES HOLDINGS LIMITED; WO2008/61108; (2008); A2;,
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. 59528-27-7, name is (4-Iodophenyl)methanamine hydrochloride, A new synthetic method of this compound is introduced below., Recommanded Product: 59528-27-7

General procedure: The aldehyde (1 mmol) and 4-iodobenzylamine hydrochloride (0.270 g, 1 mmol) were mixed with dry DCE (25 mL). If indicated, TEA (139 muL, 1 mmol) was added to liberate the parent amine. Next, Na(AcO)3BH (0.318 g, 1.5 mmol) was added and the mixture was stirred at rt for 24-36 h. Aq NaOH-soln (2 M) was added and the mixture was stirred vigorously for 10 min, after which DCM was added. The organic layer was separated and the aq layer was back-extracted with DCM (1×). The combined organic layers were dried (Na2SO4), filtered and concentrated. If required, the crude product was purified by column chromatography.

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:
Article; Wijtmans, Maikel; Verzijl, Dennis; Bergmans, Serge; Lai, Michael; Bosch, Leontien; Smit, Martine J.; De Esch, Iwan J.P.; Leurs, Rob; Bioorganic and Medicinal Chemistry; vol. 19; 11; (2011); p. 3384 – 3393;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 755027-18-0, A common heterocyclic compound, 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, molecular formula is C7H6BrIO, 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 a mixture of the product from Step 1, -bromo-4-iodo-2-methoxybenzene (750 mg, 2.4 mmol), CsF (1.09 g, 7.2 mmol), (2-amino-4-cyanophenyl)boronic acid hydrochloride (390 mg, 2.4 mmol), and Pd(PPh3)4 (277 mg, 0.24 mmol) was added DME (15 mL) under nitrogen. It was then heated to 100C. After 36 hours, EtOAc and water were added to the resulting thick red suspension. The organic layer was washed with brine, dried over Na2SO4, and the solvent was removed in vacuo. The residue was purified on silica (gradient EPO elution, 3-50% EtO Ac/hex anes) to yield the title compound as a red oil. LRMS (M+H)+ =303.1.

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

Reference:
Patent; MERCK & CO., INC.; WO2008/57208; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 364-75-0, These common heterocyclic compound, 364-75-0, name is 1-Fluoro-4-iodo-2-nitrobenzene, 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 3-3-1 Preparation of 4-iodo-N-(3-methoxy-4-((4-methoxybenzyl)oxy)benzyl)-2-nitroaniline To a stirred solution of 3-methoxy-4-((4-methoxybenzyl)oxy)phenyl)methanamine (5.02 g, 18.37 mmol) in acetonitrile (75 mL) was added 1-fluoro-4-iodo-2-nitrobenzene (4.67 g, 17.49 mmol) and diisopropylethylamine (2.83 g, 21.86 mmol). The resulting bright yellow solution was heated to reflux. After 17 h, the orange mixture was allowed to cool to room temperature and was diluted with water. The mixture was extracted with dichloromethane (3*100 mL). The combined organic phases were dried over magnesium sulfate, filtered, and concentrated to provide 9.49 g (>100%) of 4-iodo-N-(3-methoxy-4-((4-methoxybenzyl)oxy)benzyl)-2-nitroaniline as an orange semi-solid.

Statistics shows that 1-Fluoro-4-iodo-2-nitrobenzene is playing an increasingly important role. we look forward to future research findings about 364-75-0.

Reference:
Patent; KANE, JR., John L.; MATTHEWS, Gloria; METZ, Markus; KOTHE, Michael; LIU, Jinyu; SCHOLTE, Andrew; US2015/158847; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 101066-87-9, These common heterocyclic compound, 101066-87-9, name is 4-Iodo-2-(trifluoromethyl)benzonitrile, 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: A mixture of 4c (6.0 g, 24.7 mmol), 4-iodo-2-(trifluoromethyl)benzonitrile (8.42 g, 28.4 mmol), Xantphos (2.14 g, 3.70 mmol),Pd2(dba)3 (1.13 g, 1.23 mmol) and Cs2CO3 (12.05 g, 36.98 mmol)in toluene (70 ml) was stirred at 80 C for 18 h, and the resultingmixture was partitioned between water and ethylacetate. Theorganic layer was dried over MgSO4, and concentrated in vacuo.The residue was purified by silica gel column chromatography(n-hexane:EtOAc = 50:1 to 1:2) to afford 4-((2S,3S)-3-{[tert-Butyl(dimethyl)silyl]oxy}-2-ethyl-5-oxopyrrolidin-1-yl)-2-(trifluoromethyl)benzonitrile

The synthetic route of 101066-87-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Aikawa, Katsuji; Asano, Moriteru; Ono, Koji; Habuka, Noriyuki; Yano, Jason; Wilson, Keith; Fujita, Hisashi; Kandori, Hitoshi; Hara, Takahito; Morimoto, Megumi; Santou, Takashi; Yamaoka, Masuo; Nakayama, Masaharu; Hasuoka, Atsushi; Bioorganic and Medicinal Chemistry; vol. 25; 13; (2017); p. 3330 – 3349;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 755027-18-0, 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 755027-18-0 as follows.

in a sealable reaction tube was added i-brorno-4-iodo-2-rnethoxybenzene (2461 mg, 7.86 mrnol). tert-butyl I -oxo-2.8-diazaspiro[4.5] decane-8-carboxyiate (1000 mg, 3.93 mrnol), cesium carbonate (2562 mg, 7.86 rnrnol) and dioxane (7864 il). The reaction was purged with nitrogen. Then 9,9-dimethyi-4,5- bis(diphenyiphosphino)xanihene (341 rng, 0.590 mmol), Pd2(dba)3 (180 rng, 0.197 mrnoi)was added and nitrogen was bubbled through reaction for I mm. The reaction wassealed and stirred at 100 C overnight. The reaction was partitioned between EtOAc(50 ml) and water (30 ml). The organic layer was separated, washed with water (2 x 30m1) and brine (30 ml). dried over MgSO4, filtered and concentrated. The residue was purified using ISCO system (0-100% EtOAc/Hex gradient) to give tert-butyl 2-(4-bromo-3- rnethoxvphenyi)-i-oxo-2,8-diazaspiro[45]decane-8-carboxyiate (1.6 g, 364 mrnoi, 93 %yield) as a beige solid. ?H NMR (500MHz, DM50-do) d 7.67 (d, .J=2.2 Hz, 1H), 755(d, J=8.5 Hz, IH), 7.12 (dd, J=8.8, 2.5 Hz, 1H), 3.96 – 3.78 (m, 7H), 3.10 -2.84 (rn, 2H),2.10 (t. J=6.9 Hz, 21-1), 1.62 (dd, J=12.0, 4.0 Hz. 21-1), 1.51 (d, J=i3.5 Hz, 2F1), 1.42 (s,9H). MS (ESI) m/-: 43c.0, 441.0 (M+H).

According to the analysis of related databases, 755027-18-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ZHU, Yeheng; DEWNANI, Sunita, V.; EWING, William, R.; (265 pag.)WO2019/89868; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 628-21-7, name is 1,4-Diiodobutane, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C4H8I2

General procedure: At room temperature and under nitrogen atmosphere, 12.5 mmol of menthol in 25 mL of THF was added dropwise to a solution containing 24.4 mmol of oil-free KH suspended in 25 mL of THF. When hydrogen evolution had ceased, the reaction mixture was cooled to -50 C and 12.5 mmol of TCE dissolved in 15 mL of THF was slowly added. Once the addition was completed, the cooling bath was removed and the solution was stirred for 1 h at room temperature. The reaction mixture was then cooled to -78 C and a freshly titrated solution of BuLi (30.0 mmol) was added dropwise. After stirring for 30 min at -78 C and 30 min at -50 C, 40.5 mmol of HMPA was added. After stirring for 15 min, the following solution was added: 25 mmol of diiodoalkane (diiodobutane or diiodopentane) in 5.4 mL of THF. The cooling bath was removed and stirred at room temperature for 24 h under nitrogen atmosphere. The solution was then treated with 15 mL of water. The layers were separated. The aqueous phase was extracted thrice with hexanes. The combined organic layers were successively washed with water and brine, and dried over anhydrous MgSO4. Crude product was then purified with flash chromatography using hexanes as eluent.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 628-21-7.

Reference:
Article; Hanna, Rana; Daoust, Benoit; Tetrahedron; vol. 67; 1; (2011); p. 92 – 99;,
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. 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H9IO2

Under protective gas A-Ia (0.2 g, 0.724 mmol) together with bis-triphenylphosphine- palladium dichloride (25.4 mg, 0.036 mmol) and copper(I)iodide is added to abs. THF (3 mL) and triethylamine (1 mL). Trimethylsilyl-ethyne is added at RT to this reaction mixture and stirred overnight. For working up it is diluted with EE, poured onto 0.5 M ammonia solution and the aqueous phase is again extracted with EE. The combined organic phases are washed with 0.5 M hydrochloric acid and saturated NaCl solution, extracted again with EE, dried on sodium sulphate, filtered and evaporated down under reduced pressure.The residue is combined with methanolic KOH (1 mL) and stirred for 2 h at RT. The reaction mixture is diluted with EE, poured onto 5 % NaHCO3 solution and extracted twice with EE. The combined organic phases are washed with saturated sodium chloride solution, dried on sodium sulphate, filtered and evaporated down under reduced pressure. Chromatographic purification through a short silica gel frit yields A-2a (HPLC-MS: tRet. = 3.65 min; MS (M+H)+ = 175).

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; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WO2009/3998; (2009); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 41860-64-4,Some common heterocyclic compound, 41860-64-4, name is 4-Fluoro-2-iodo-1-nitrobenzene, molecular formula is C6H3FINO2, 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. 5-Fluoro-4′-Methylsulfinyl-2-Nitrobiphenyl sulfide 4-Methylsulfinylthiophenol (0.2 mole) is dissolved in dry tetrahydrofuran (100 ml.) and sodium hydride (50% dispersion in mineral oil, 0.2 mole) is added over 30 minutes. The solution is evaporated to dryness and the residue is rinsed well with n-hexane. The powdered salt is stirred under N2 at reflux with 4-fluoro-2-iodonitrobenzene (0.2 mole) in dry dimethylformamide for 16 hours, evaporated to dryness and extracted into chloroform (3 times 200 ml.). The organics are washed with water (2*100 ml.), separated and dried (MgSO4). The solution is filtered, evaporated to dryness and put on a column of silica-gel (Baker 2 in. times 2 ft.) and various fractions are eluted with portions of benzene-n-hexane. In this way, pure 5-fluoro-4′-methylsulfinyl-2-nitrobiphenyl sulfide is obtained.

The synthetic route of 41860-64-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Cell Pathways, Inc.; US6020379; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com