Tag: M.W=200-300

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. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Iodo-1,3-dimethoxybenzene

Isopropylmagnesium chloride (10 mL, 10mmol) was added to the THF solution (60 mL) ofthe compound 1 (g [ 5.28 ], 20mmol), and it stirred at the room temperature for 1 hour. Then,the phosphorus trichloride (1.7 mL, 25mmol) was added at 78 degree C, and it stirred at theroom temperature for 2 hours. After removing a solvent and an excessive phosphorustrichloride under decompression, THF (50 mL) was added and the solution containing thecompound 2 was obtained.

According to the analysis of related databases, 16932-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JAPAN POLYETHYLENE CORPORATION; JAPAN POLYPROPYLENE CORPORATION; XIN, SHIXUAN; SHIMIZU, FUMIHIKO; SATO, NAOMASA; TANNA, AKIO; (45 pag.)JP5812764; (2015); B2;,
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 124700-40-9 as follows. Application In Synthesis of 2-Fluoro-4-iodobenzoic acid

2-Fluoro-4-iodobenzoic acid (61) (5.35 g, 20.1 mmol) was dissolved in methanol (30 mL, 741 mmol) was added thionyl chloride (2.6 mL, 35.8 mmol), dropwise at 0 C. with stirring. The reaction solution was then refluxed in an oil bath at 85 C. for 1 hour. Excess methanol was removed in vacuo, and benzene (20 mL) was added to the residue and then removed in vacuo. To the residue was added ethyl acetate (150 mL), and the organic layer was washed with saturated NaHCO3 (200 mL) and brine (60 mL) and then dried over sodium sulfate, filtered and concentrated in vacuo. The crude product was purified by column chromatography (150 mL SiO2, ethyl acetate:hexanes 1:48) to give compound 62 (5.3066 g, 94%) as a white crystalline solid, m.p. 76-78 C.: 1H NMR (400 MHz, CDCl3) delta 7.63 (t, J=8.0, 1H), 7.56 (dd, J=8.4, 1.6, 1H), 7.53 (dd, J=10.0, 1.2, 1H), 3.92 (s, 3H); 13C NMR (100.6 MHz, CDCl3) delta 164.4, 164.3, 162.3, 159.7, 133.5, 133.4, 133.0, 126.5, 126.3, 118.2, 118.1, 99.8, 99.7, 52.5; IR (neat) n 2952, 1700, 1595, 1561 cm-1; LC-FAB-MS (M)+ calcd for C8H6FIO2 279.9397, found 279.9394.

According to the analysis of related databases, 124700-40-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY; Wagner, Carl E.; Marshall, Pamela A.; Jurutka, Peter W.; (35 pag.)US2018/207156; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-62-0, 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. 626-62-0, name is Iodocyclohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 2 mL crimp-top GC vial was charged with NiBr2(DME) (6.2 mg, 0.02 mmol, 0.1 equiv), dppf (11 mg, 0.02 mmol, 0.1 equiv), and activated Zn powder [35] (26.2 mg, 0.4 mmol, 2 equiv). The vial was crimped shut and the olefin (0.2 mmol, 1 equiv) was injected through the septum as a solution in 0.3 mL THF followed by 0.2 mL HFIP. The iodide (1-2 equiv) was then added (as a solution in THF, if solid) and the vial was shaken at 1000 rpm for 12 h at 25 C. The reaction was diluted with EtOAc and quenched by the addition of 1 M HCl (aq). The aqueous phase was extracted with three portionsof EtOAc. The combined organic phase was then passed through a plug of silica. An aliquot of the organic phase was used for GC or GC/MS analysis with mesitylene as an internal standard. Solvent was removed and the mixture was purified by chromatography on silicagel with EtOAc/hexane as the eluent to give the products as colorless oils.

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

Reference:
Article; Diccianni, Justin B.; Chin, Mason; Diao, Tianning; Tetrahedron; vol. 75; 31; (2019); p. 4180 – 4185;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

58313-23-8, name is Ethyl-3-iodobenzoate, 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. Recommanded Product: Ethyl-3-iodobenzoate

Synthesis of 3-[2-Oxo-3-(l-phenyl-ethylidene)-2,3-dihydro-indol-l-yl]-benzoic acid ethyl ester; A Schlenk tube was charged with Cul (9.6 mg, 0.050 mmol, 5.0 mol %), 3-(l-Phenyl- ethylidene)-l,3-dihydro-indol-2-one (352.7 mg, 1.5 mmol), and K2C03 (276 mg, 2.0mmol), evacuated, and backfilled with argon. N, TV-Dimethylethylenediamine (11 uL, 0.10 mmol, 10 mol %), ethyl 3-iodobenzoate (278.8 mg, 1.01 mmol), and acetonitrile (1.5 ml) were added under argon. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at 80 C for 23 h. HPLC monitor the reaction finished. Remove the solvent under reduced pressure. The residue was separated by flash chromatography column(gradient elution, 5-10% ethyl acetate in petroleum ether) to give 3-[2-Oxo-3-(l- phenyl-ethylidene)-2, 3 -dihydro-indol-l-yl] -benzoic acid ethyl ester as yellow powder (344 mg, 90%). 1H NMR (400 MHz, CDC13) 5ppm 1.42 (t, j=7.20 Hz, 3 H) 2.87 (s, 3 H) 4.42 (q, J=7.07 Hz, 2H) 6.25 (d, J=7.58 Hz, 1 H) 6.68 – 6.78 (m, 2 H) 7.09 (t, j=7.71 Hz, 1 H) 7.34 – 7.40 (m, 2 H) 7.47 – 7.58 (m, 3H) 7.62 – 7.72 (m, 2 H) 8.11 – 8.19 (m, 2 H) . MS calcd. for C25H2iN03 383, obsd. (ESf) [(M+H)+] 383.9.

The synthetic route of 58313-23-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; NAN, Fajun; YU, Lifang; ZHANG, Mei; CHEN, Li; HUANG, Mengwei; FENG, Lichun; LI, Jia; PANG, Tao; WO2011/32320; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 170112-66-0, name is 3,4,5-Trifluoroiodobenzene, molecular formula is C6H2F3I, 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. Safety of 3,4,5-Trifluoroiodobenzene

Method for preparing ethyl 2,2-difluoro-2- (3,4,5-trifluorophenyl) acetate 3,4,5-trifluoroiodobenzene (10.0 g, 38.0 mmol),Ethyl bromodifluoroacetate (23.1 g, 114 mmol)And a solution of copper (2.90 g, 45.6 mmol) in dimethylsulfoxide (40 ml)Was stirred at 80 C. for 3 hours. Ethyl acetate was added to the reaction mixture, and insoluble matter was filtered off. Pour water into the filtrate,And extracted with ethyl acetate. The extract was washed with saturated brine,After drying with anhydrous sodium sulfate,And concentrated under reduced pressure. The concentrate was purified by silica gel column chromatography (elution solvent: ethyl acetate / n-hexane = 1/10) to give the title compound as a colorless oil (yield 7.20 g, yield 75%). J = 7.3 Hz), 1.31 (3H, t, J = 7.3 Hz), 1 H NMR spectrum (CDCl 3) sigma: 7.26 (2H, t, J = 6.9 Hz), 4.31 ).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 170112-66-0, its application will become more common.

Reference:
Patent; Hokko Chemical Industry Co., Ltd.; Suzuki, Jun; Kobayashi, Yuta; Murakami, Hideyuki; Ono, Ryuta; Onoue, Shinji; Ota, Shinya; Nonaka, Hisato; (29 pag.)JP2016/84347; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 335349-57-0, name is 5-Chloro-4-iodo-2-nitroaniline, 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. SDS of cas: 335349-57-0

To a mixture of 5-chloro-4-iodo-2- nitroaniline 1-5 (31.7 g, 106 mmol) and iron powder (59.0 g, 1060 mmol) in 880 mL ethanol was added a solution OfNH4Cl (28 g, 530 mmol) in 240 mL of water. The resulting mixture was mechanically stirred at 60 C for 40 h. After cooling to rt the mixture was filtered and the filtrate reduced to about 500 mL by rotary evaporation. This filtrate was diluted with 1 L of EtOAc and I L of water, and shaken. The organic layer separated, washed with brine, dried (MgSO4) and evaporated to provide crude product. The crude product was dissolved in 80 mL of EtOAc, diluted with 80 mL of hexanes and injected onto a 330 g column Of SiO2, which was pre-eluted with 33% EtOAc in hexanes. The column was subjected to MPLC eluting at 100 mL/min with 33% EtOAc in hexanes (15 min) and then 50% EtOAc (20 min) to provide 5-chloro-4-iodo-l,2- phenylenediamine 1-6. Impure fractions of residue were resubjected to MPLC on a 330 g column of SiO2 by the same method to provide additional 5-chloro-4-iodo-l ,2-phenylenediamme 1-6 as an amorphous solid. 1H NMR (500 MHz, DMSO-d6): delta 4.77 (s, 2H), 4.91 (s, 2H), 6.66 (S5 IH), 6.93 (s5 IH); LC-MS: calculated for C6H6ClIN2 267.9, observed m/e 269.0 (M + H)+.

The synthetic route of 5-Chloro-4-iodo-2-nitroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; METABASIS THERAPEUTICS, INC.; BOOKSER, Brett, C.; DANG, Qun; GIBSON, Tony, S.; JIANG, Hongjian; CHUNG, De Michael; BAO, Jianming; JIANG, Jinlong; KASSICK, Andy; KEKEC, Ahmet; LAN, Ping; LU, Huagang; MAKARA, Gergely, M.; ROMERO, F., Anthony; SEBHAT, Iyassu; WILSON, David; WODKA, Dariusz; WO2010/47982; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 620621-48-9, A common heterocyclic compound, 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, molecular formula is C8H6ClIO2, 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.

107.1 2-chloro-5-(pyridin-3-yloxy)benzoic acid methyl ester A microwave vial was charged with copper (I) bromide (7.7 mg), Cs2CO3 (685 mg), 3-hydroxypyridine (100 mg) and methyl-2-chloro-5-iodobenzoate (374 mg) and flushed with argon. DMSO (1.6 mL) was added followed by 2-pyridyl acetone (0.014 mL) and the reaction mixture was heated to 100 C. for 3 h in the microwave. It was diluted with EtOAc, filtered and the filtrate was washed with H2O. The organic phase was dried over MgSO4 and concentrated in vacuo. The crude was purified by CC (Hept/EtOAc 1/0 to 1/1) to give 58 mg of the titled compound as a yellowish waxy solid. LC-MS (B): tR=0.59 min; [M+H]+: 264.26

The synthetic route of 620621-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Actelion Pharmaceuticals Ltd.; Hilpert, Kurt; Hubler, Francis; Murphy, Mark; Renneberg, Dorte; US2014/73651; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 2468-56-6, 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. 2468-56-6 name is 6-Iodohex-1-yne, 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: Concentrated sulfuric acid (0.15 mL) was added under stirring at ambient temperature to a suspension of 25 mmole of uracil 3 or uracil derivatives, namely 6-methyluracil 4, thymine 5, quinazoline-2,4(1H,3H)-dione 6 and hexamethyldisilazane (HMDS, 62.5 mmol) in 100 mL of toluene. The mixture was refluxed for 4 h, the solvent and excessive HMDS were removed to afford bis(trimethylsilyl) ether derivative 7. This crude product was engaged in the next step without any previous purification. A solution of 40 mmole of appropriate alkyne (propargyl bromide, 5-iodo-1-pentyne, 6-iodo-1-hexyne) in DMF (3 mL) was added to the crude product 7 and the reaction mixture was stirred at 115-130 C for 12 h. After the solvent was distilled off under reduced pressure, 200 ml of chloroform was added to the residue, and the mixture was filtered. The filtrate was concentrated, and the residue was purified by column chromatography on silica gel using as eluent first petroleum ether, then petroleum ether-ethyl acetate (1.5:1) and then ethyl acetate. From the third fraction the target N1-alkynyl-3,4-dihydro-2,4-dioxopyrimidines (3a,b, 4b,c, 5a,b, 6a,b) were isolated.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 6-Iodohex-1-yne, and friends who are interested can also refer to it.

Reference:
Article; Andreeva, Olga V.; Belenok, Maya G.; Saifina, Liliya F.; Shulaeva, Marina M.; Dobrynin, Alexey B.; Sharipova, Radmila R.; Voloshina, Alexandra D.; Saifina, Alina F.; Gubaidullin, Aidar T.; Khairutdinov, Bulat I.; Zuev, Yuriy F.; Semenov, Vyacheslav E.; Kataev, Vladimir E.; Tetrahedron Letters; vol. 60; 47; (2019);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 2401-21-0, A common heterocyclic compound, 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, molecular formula is C6H3Cl2I, 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 97 d-1-(4′-Amino-3′-chloro-5′-fluoro-phenyl)-2-tert.butylamino-ethanol 0.26 gm of d-1-(4′-amino-3′-fluoro-phenyl)-2-tert.butylamino-ethanol hydrochloride and 0.2 ml of pyridine were dissolved in 30 ml of tetrahydrofuran, and the solution was cooled to 0¡ã C. 0.3 gm of iodobenzene dichloride were added, the mixture was held at 0¡ã C. for 2 hours, and then 0.1 gm of iodobenzene dichloride was added again. After standing for 20 hours at about 4¡ã C. the solution was evaporated, and the residue was distributed between ethyl acetate and water. The aqueous phase was made alkaline with 2N ammonia and was then extracted again with ethyl acetate. The organic phase was washed with water, dried and evaporated to dryness in vacuo. The residue was dissolved in absolute ethanol, the solution was neutralized with ethanolic hydrochloric acid, and the hydrochloride of the above-named compound was caused to crystallize by addition of ether. M.p. 210¡ã-211¡ã C. (decomp.). [alpha]36420 = +139.6¡ã (c = 2.0; methanol).

The synthetic route of 2401-21-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Boehringer Ingelheim GmbH; US4119710; (1978); A;,
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. 25309-64-2, name is 1-Ethyl-4-iodobenzene, A new synthetic method of this compound is introduced below., SDS of cas: 25309-64-2

(39-1) Synthesis of 3-(4-ethylphenyl)-2-propyne-l-ol (compound 39-1) [Show Image] A mixture of 4-ethyliodobenzene (5.00 g), copper(I) iodide (82.1 mg), triphenylphosphine (283 mg), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (446 mg), propargyl alcohol (1.40 ml), diisopropylethylamine (15.0 ml) and tetrahydrofuran (100 ml) was stirred at room temperature for 12 hr. The reaction mixture was added to water, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=98:2 – 80:20) to give the object product (2.10 g) as a brown oil. 1H-NMR(CDCl3) delta (ppm): 1.23(3H, t, J=7.6Hz), 1.65(1H, t, J=6.0Hz), 2.64(2H, q, J=7.6Hz), 4.49(2H, d, J=5.9Hz), 7.15(2H, d, J=7.6Hz), 7.36(2H, d, J=7.6Hz).

The synthetic route of 25309-64-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; EP2168944; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com