Month: April 2021

Related Products of 135050-44-1, 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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a deoxygenated solution of 3-chloro-4-iodo-aniline (6.95 g), triphenyl arsine (0.67 g), and tris(dibenzylideneacetone)palladium(0) (0.50 g) in tetrahydrofuran (120 mL) at 50 C is added tributylvinyltin (10 g) and the mixture is stirred for approximately 15 hours at 50 C under an atmosphere of argon. The reaction is then cooled, filtered through diatomaceous earth, and the filtrate is evaporated to dryness under reduced pressure. The residue is dissolved in hexanes and then extracted three times with 5% aqueous hydrochloric acid. These aqueous acidic extracts are then basified with solid potassium carbonate and extracted three times with ethyl acetate. These pooled organic extracts are then washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and the solvent is removed under reduced pressure. The resulting residue is chromatographed over silica gel (hexanes and then 10% ethyl acetate in hexanes is used as the eluant) to provide the desired product as an amber oil.

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-Chloro-4-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wyeth; EP1137645; (2004); 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. 103440-54-6, name is Methyl 5-iodo-2-methylbenzoate, A new synthetic method of this compound is introduced below., Recommanded Product: 103440-54-6

A solution of compound 7 (39.6 g, 0.143 mol) and 1-vinyl-2-pyrrolidinone (18.5 g, 0.143 mol) in anhydrous THF (200 mL) was added slowly to a gently refluxing suspension of sodium hydride (9.2 g, 60% in mineral oil, 0.229 mol) in THF (70 mL). After the addition, the mixture was stirred at reflux for additional 3 hours. TLC (petroleum ether: ethyl acetate = 10:1) showed the reaction was complete. The mixture was cooled and the excess sodium hydride was EPO quenched with saturated aqueous ammonium chloride. The mixture was concentrated in vacuo to remove THF. The residue was extracted with ethyl acetate (400 ml_x2). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give crude product 8, which was used in the next step without further purification.

The synthetic route of 103440-54-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER INC.; WO2006/117669; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 755027-21-5, 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. 755027-21-5 name is 4-Chloro-1-iodo-2-methoxybenzene, 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.

A dry round bottomed flask was charged with KOTBU (1.903 g, 17.0 mmol), 5-chloro- 2-iodoanisole (4.054 g, 15.1 mmol), Pd2dba3 (144 mg, 0.16 mmol), DPEPhos (176 mg, 0.33 mmol) and 3-FLUORO-THIOPHENOL (1.903 g, 17.0 mmol). The flask was evacuated and BACKFILLED with Ar three times. Dry toluene (80 mL) was added and the mixture stirred at 95 C for 2 h. The mixture was filtered through a pad of silica gel followed by adsorption onto silica gel. After purification by flash chromatography using silica gel, eluting with heptanes/EtOAc, 97: 3, the title compound was obtained as a yellow oil (3.41 g, 85%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-1-iodo-2-methoxybenzene, and friends who are interested can also refer to it.

Reference:
Patent; H. LUNDBECK A/S; WO2004/96761; (2004); 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. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,2-Dichloro-4-iodobenzene

General procedure: A mixture of an appropriate unnatural amino acid carboxamide 6 (0.15-0.2 mmol, 1 equiv), an appropriate aryl iodide (5 equiv), Pd(OAc)2 (10 mol%) and AgOAc (2.5 equiv) in anhydrous toluene (2-3 mL) was heated at 110 C for 15-24 h under a nitrogen atm or in a sealed tube. After the reaction period, the reaction mixture was concentrated under reduced pressure to afford a crude reaction mixture, which was purified by column chromatography on neutral alumina or silica gel (eluent EtOAc:hexane) to give the corresponding arylated amino acid (see the respective Schemes/Tables for the specific entries). 3.4.27. 3-(3,4-Dichlorophenyl)-6-(1,3-dioxoisoindolin-2-yl)-N-(quinolin-8-yl)hexanamide (10c). The compound 10c was obtained after purification by column chromatography on silica gel (EtOAc:hexane 40:60) as a greencolor solid (60 mg, 75%); Rf (40% EtOAc/hexane) 0.7; mp:110e112 C; IR (DCM): 3346, 2937, 1771, 1394, 723 cm1; 1H NMR(400 MHz, CDCl3) dH 9.64 (1H, br. s), 8.78 (1H, d, J 3.2 Hz), 8.65(1H, t, J 4.5 Hz), 8.15 (1H, d, J 7.7 Hz), 7.81 (2H, dd, J1 5.2,J2 3.1 Hz), 7.70 (2H, dd, J1 5.4, J2 3.1 Hz), 7.49 (2H, d, J 4.6 Hz),7.46 (1H, dd, J1 8.3, J2 4.2 Hz), 7.39 (1H, d, J 1.4 Hz), 7.32 (1H, d,J 8.2 Hz), 7.13 (1H, dd, J1 8.2, J2 1.5 Hz), 3.67 (2H, t, J 7.3 Hz),3.36e3.29 (1H, m), 2.87 (1H, dd, J1 14.8, J2 6.4 Hz), 2.80 (1H, dd,J1 14.8, J2 8.3 Hz), 1.92e1.82 (1H, m), 1.78e1.65 (2H, m),1.60e1.52 (1H, m); 13C NMR (CDCl3, 101 MHz): dC 169.2, 168.3,148.1,143.9, 138.2, 136.3, 134.1, 133.9, 132.7, 132.0, 130.6, 130.6, 129.4,127.9, 127.3, 127.2, 123.2, 121.6, 121.6, 116.5, 45.1, 41.6, 37.7, 33.2,26.5; HRMS (ESI) calcd for C29H24Cl2N3O3 [MH] 532.1195 found532.1177.

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; Tomar, Radha; Bhattacharya, Debabrata; Babu, Srinivasarao Arulananda; Tetrahedron; vol. 75; 17; (2019); p. 2447 – 2465;,
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. 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H4ClIO2

General procedure: To a stirred solution of the corresponding benzoic acid (1.0 equiv) in dry MeOH (2.0 mL per 1.0 mmol of benzoic acid) at 0 C. was added SOCl2 (2.0 equiv) dropwise. After addition, the reaction was allowed to stir at room temperature overnight. The crude reaction was concentrated in vacuo, quenched with water, and extracted with EtOAc. The combined organic layer was washed with saturated aqueous NaHCO3, dried over anhydrous Na2SO4, concentrated by rotary evaporation, and purified by column chromatography to give 21a-b.

According to the analysis of related databases, 13421-13-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jorgensen, William L.; Anderson, Karen S.; US2015/105351; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 54811-38-0, The chemical industry reduces the impact on the environment during synthesis 54811-38-0, name is 5-Iodo-2-methylbenzoic acid, I believe this compound will play a more active role in future production and life.

Borane-methylsulfide solution (50.0 mL of a 2.0M solution in THF, lOOmmol) was added dropwise to a solution of 5-iodo-2-methyl benzoic acid (13.1g, 50 mmol) and anhydrous THF (100 mL) at 35-45 C at a rate to moderate the gas evolution. The resulting mixture was heated at 60 C for 3 h and was then cooled to 25 C and quenched by the careful, dropwise addition of methanol (50 mL) which was added at such a rate that gas evolution was moderated and the temperature was maintained below 35 C. The resulting mixture was stirred at 25 C for 2 h and was then concentrated under vacuum. The residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution, the organic phase was washed with saturated aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and concentrated to provide the title compound (11.58 g) as a white solid H NMR (CDCI3) delta 7.71 (d, 1H), 7.52 (d, 1H), 6.91 (d, 1H), 4.64 (s, 2H), 2.27 (s, 3H), 1.62 (br s, 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, 5-Iodo-2-methylbenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; TAGGI, Andrew, Edmund; DIETRICH, Robert, F.; MARCUS, Kimberly, Katherine; MCCANN, Stephen, Frederick; WO2014/66120; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 619-58-9,Some common heterocyclic compound, 619-58-9, name is 4-Iodobenzoic acid, 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 test tube containing a magnetic bar was added aryl iodide(1 mmol), copper powder (6.35 mg, 0.1 mmol), Na2S¡¤9H2O(720.54 mg, 3 mmol), and DMSO (2 mL). After flushing withargon, 1,2-ethanedithiol (8.4 muL, 0.1 mmol) was added. Themixture was stirred in the oil bath at 100 C for 20 h. Aftercooled to ambient temperature, the reaction mixture was distributedin aq HCl (5%) and EtOAc. The organic layer was separated and washed with water and brine, dried, and concentratedunder vacuum. The crude product was further purifiedby column chromatography using ethyl acetate/n-hexane aseluent to provide the desired aryl thiol.

The synthetic route of 619-58-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Xue, Hongyu; Jing, Bing; Liu, Shasha; Chae, Junghyun; Liu, Yajun; Synlett; vol. 28; 17; (2017); p. 2272 – 2276;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 191348-14-8,Some common heterocyclic compound, 191348-14-8, name is 2-Iodo-4-methoxyaniline, molecular formula is C7H8INO, 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 anhydrous and anaerobic conditions, 0.1 mmol of 2-iodo-4-methoxyaniline was added.0.12 mmol of benzaldehyde, 0.3 mmol of selenium powder, 0.005 mmol of copper, 0.2 mmol of potassium hydroxide and 10 ml of DMSO solution were refluxed at 120 C in a single-neck round bottom flask, and the reaction was monitored by TLC.Separation of pure methoxy-containing benzoselenazole compounds by column chromatographyThe reaction product was obtained by demethylation of boron tribromide (3 eq.).The product was a white solid with a yield of 39%.

The synthetic route of 191348-14-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wuhan University; Zhou Haibing; Zhang Silong; Hu Zhiye; Li Yuanyuan; Ning Wentao; Dong Chune; (13 pag.)CN108863985; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 886762-71-6, name is 1-Fluoro-3-iodo-2-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. name: 1-Fluoro-3-iodo-2-nitrobenzene

K2CO3 [5.20 g, 37.7mmoi] was added to a stirred suspension of compound 3 [7.0 g, 34 mmol] in EtOH (230 mL) under ice cold condition. After addition reaction mixture was left to stir vigorously for half an hour under cold condition. Finally, compound 2 [9.16 g, 34.3 mmol] was added portion wise to the reaction mixture at 0 C, after addition reaction mixture was brought to room temperature and heated at 80 C for 40 h. After completion, EtOH were evaporated, crude was diluted with water [200 mL] and extracted with EI2O [200 L] Organic part was separated; pH of the aqueous part was slowly adjusted to 2-3 using 1 (N) aqueous HC1 under ice cooled condition and immediately extracted with EtOAc [2×200 mL] Organic part was separated, dried [MgSOr] and concentrated under reduced pressure to afford compound 4 [10.6 g, 68 4 %] as dark red floppy solid. Mass [ESI]: ra/z 451.21 j .1 – l 1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 886762-71-6, its application will become more common.

Reference:
Patent; CYTOSITE BIOPHARMA INC.; BILCER, Geoffrey, Malcolm; KELLY, Terence, Alfred; (190 pag.)WO2019/160916; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 35453-19-1, The chemical industry reduces the impact on the environment during synthesis 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, I believe this compound will play a more active role in future production and life.

5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol) (commercially available from Aldrich), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1 ,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during 11/4 to 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 500C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product. 13C NMR (DMSOd6) 66, 78.4, 148.9, 149.2, 169 MS (ES-) found 593.5 [M-H+], expected 593.7

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, 5-Amino-2,4,6-triiodoisophthalic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GE HEALTHCARE AS; WO2008/123779; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com