Category: iodides-buliding-blocks

These common heterocyclic compound, 260558-15-4, name is 4-Bromo-2-iodo-1-methylbenzene, 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. Safety of 4-Bromo-2-iodo-1-methylbenzene

A dry flask was charged with 4-BROMO-2-IODO-1-METHYL-BENZENE (6.85 G, 23.1 MMOL) and the flask was evaporated and then filled with argon and this process repeated twice. Dry THF (20 mL) was added, and the solution cooled to-35 C ; then isopropylmagnesium chloride (11.5 mL, 2.0 M in diethyl ether, 23 MMOL) was added slowly over 40 min keeping the temperature below-35 C. On completion of the addition the reaction mixture was stirred at-35 C for 30 min. A THF solution of ZNCI2 (3.93 G, 28. 9 mmol, 0.7 M) was added dropwise over 20 min. The reaction mixture was stirred at 0 C for 20 min; then 2-chloro-4-nitro-benzoyl chloride (5.33 g, 24.2 MMOL) and Cu (OAC) Z (92 mg, 0.46 MMOL) were added and the reaction mixture was allowed to warm to room temperature. After 16 h the reaction mixture was poured into a mixture of ETOAC/WATER, then shaken and separated. The aqueous phase was extracted with more EtOAc. The organic phases were combined, dried (MGS04), filtered, and concentrated in vacuo to afford the crude product. The crude product was purified by flash chromatography using EtOAc/petroleum ether 1: 14 as the eluent to give the title compound as almost white solid.

The synthetic route of 4-Bromo-2-iodo-1-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LEO PHARMA A/S; WO2005/9940; (2005); A1;,
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 1133123-02-0 as follows. Computed Properties of C7H4BrIO2

General procedure: A sealed tube was charged with CuCl (0.02 mmol), BFMO (0.02 mmol), N-protected N-alkenylhydrazine (2.0 mmol), 2-iodobenzoic acid (2.4 mmol), and K2CO3 (4 mmol). The tube was evacuated and backfilled with argon three times before anhydrous DMSO (4.0 mL) was added via syringe (NOTE: for liquid substrates, they were added into the tube via syringe after the tube was backfilled with argon). The mixture was sealed and stirred at 80 C for 24 h. The mixture was diluted with EtOAc, washed with water, dried over anhydrous sodium sulfate, and filtrated. The filtrate was concentrated in vacuo and the residue was treated with 4M HCl/1,4-dioxane (1.2 mL) at 80 C. After the starting material was completely consumed, the solution was cooled and diluted with EtOAc. The resultant mixture was washed with water and dried over anhydrous sodium sulfate. After the solution was concentratedin vacuo, the residue was purified by flash chromatography to afford the corresponding indole.

According to the analysis of related databases, 1133123-02-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Wei, Quanpeng; Wang, Yunhan; Zhao, Jinlong; Zhang, Xiaojing; Ma, Dawei; Tetrahedron; vol. 76; 1; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

19099-54-8, name is 1-Iodo-2-isopropylbenzene, 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: 19099-54-8

General procedure: A DMF solution (8mL) of the o-substituted aryl iodide (0.36mmol), the o-bromobenzyl alcohol (0.36mmol) and norbornene (34mg, 0.36mmol) was added under nitrogen to a Schlenck-type flask, containing Pd(OAc)2 (4mg, 0.018mmol), the phosphine (0.036mmol), when required, and K2CO3 (124mg, 0.90mmol) or CsOPiv (211mg, 0.90). The reaction mixture was stirred at 105C for 24h. After cooling to room temperature the organic layer was diluted with EtOAc (20mL), washed twice with water (20mL) and dried over Na2SO4. The solvent was removed under reduced pressure and the resulting residue was purified by flash chromatography on silica gel using mixtures of hexane-EtOAc as eluent.

The synthetic route of 19099-54-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Della Ca, Nicola; Fontana, Marco; Xu, Di; Cremaschi, Mirko; Lucentini, Riccardo; Zhou, Zhi-Ming; Catellani, Marta; Motti, Elena; Tetrahedron; vol. 71; 37; (2015); p. 6389 – 6401;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 624-76-0,Some common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, molecular formula is C2H5IO, 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.

taking theobromine 540mg (3mmoL), NaH 720mg (30mmol) dissolved in 80mL DMF, adding 2mmol of 2-iodoethanol under the drop, after 4 hours of reaction, quenching the reaction with water, spin dry, oil Ether: CH3CH2OCOCH3 = 3:1 (v/v) as a mobile phase over silica gel to give compound 1-ethylhydroxy-3-7-dimethylxanthine, yield 94%.

The synthetic route of 624-76-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan University Huaxi Hospital; Huang Wen; (18 pag.)CN109912598; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 74534-15-9, 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. 74534-15-9, name is 1-Chloro-2-iodo-4-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To an oven-dry ground test tube equipped with a stir bar were added 1 mmol 2-bromoiodobenzene, 1mmolL-alaninamide, 3 mmol potassium carbonate and 5 mL DMF. The test tube was sealed with a rubber stopperand was evacuated and refilled with argon for three times. Then the test tube was stirred in an oil bathpreheated at 90? C for 48 hours. After the test tube was cooled to room temperature, the reaction wasquenched with water, and the reaction mixture was extracted with 20 mL ethyl acetate for three times. Thecombined organic layer was washed with 10 mL water and then saturated sodium chloride aqueous solution,and dried over anhydrous sodium sulfate. After filtration, the filtrate was condensed on a rotary evaporator invacuum. The resulting crude product was chromatographed on silica gel (300-400 mesh) with a 1:2 volumeratio mixed solution of ethyl acetate and petroleum ether as eluent to give a white solid L-N-phenylalaninamide.

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-Chloro-2-iodo-4-nitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wang, Yan; Tu, Xingzhao; Lv, Xirui; Zhou, Lihong; Zeng, Qingle; Tetrahedron Letters; vol. 54; 45; (2013); p. 6045 – 6048;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 116632-39-4, 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. 116632-39-4, name is 5-Bromo-2-iodotoluene, This compound has unique chemical properties. The synthetic route is as follows.

A Schlenk tube was charged with compound 471 (4.25 G, 10.9 MMOL) in 1,4-dioxane (40 mL), 5-BROMO-1-IODO-TOLUENE (3. 88 G, 13.1 MMOL), CS2CO3 (4.97 G, 15.26 MMOL), PD2 (dba) 3 (250 mg, 0.27 MMOL), and rac-BINAP (255 mg, 0.41 MMOL). The tube was capped with a rubber septum, flushed with argon for 5 min, and then stirred at 100 C for 72 h. The reaction mixture was allowed to cool to RT, and then poured into a mixture of water and EtOAc. The aqueous phase was extracted twice with more EtOAc. The combined organic phases were washed with brine, dried (MGSO4), filtered and concentrated in vacuo. The crude product was purified by chromatography eluting with petroleum ether/EtOAc 4: 1 to afford the title compound as YELLOW FOAM. 1H NMR (CDOS) 8 7.39 (d, LH), 7. 35 – 7.25 (m,3H), 7.14 (d,1H), 6.81 (m,2H), 6.69 (m,2H), 5.63 (BS, LH), 4.70 (bt, LH), 4.23-4. 00 (m, 3H), 3.95-3. 77 (m, 2H), 3.53 (m, LH), 2. 51 (s, 3H), 2. 23 (s, 3H), 1.92-1. 45 (m, 6H)

The chemical industry reduces the impact on the environment during synthesis 5-Bromo-2-iodotoluene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; LEO PHARMA A/S; WO2005/9940; (2005); A1;,
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 624-75-9 as follows. Recommanded Product: 2-Iodoacetonitrile

To a solution of 5-chloro-2-isopropyl-4-methoxy-phenol (10.36 g, 51.6 mmol) in 40 mL DMF was added K2CO3 (8.55 g, 62.0 mmol) and the mixture was heated to 65 C. After 15 minutes iodoacetonitrile (9.05 g, 54.2 mmol) was added and the mixture was heated to 80 C. for 1 hour. The mixture was cooled, poured into an ice/H2O mixture and extracted with 1:1 toluene/hexane. The combined organics were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by passing through a short plug of silica to afford (5-chloro-2-isopropyl-4-methoxy-phenoxy)-acetonitrile (11.97 g, 97%) as a white solid.

According to the analysis of related databases, 624-75-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Roche Palo Alto LLC; US2007/49609; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 181765-86-6,Some common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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 mixture of methyl 5-bromo-2-iodobenzoate (300 mg, 0.880 mmol), aniline (115 mg, 1.23 mmol), Pd2(dba)3(8.1 mg, 0.0088 mmol), Xantphos (10.2 mg, 0.0176 mmol), and Cs2C03(401 mg, 1.23 mmol) suspended in anhydrous dioxane (1.5 mL) was heated at 100 C under N2atmosphere for 16 hours. The reaction mixture was diluted with EtOAc (100 mL) and washed with brine (100 mL). The organic phase was dried over anhydrous Na2S04and concentrated under reduced pressure. Purification by flash column chromatography (hexanes to 80:20 hexanes/EtOAc) afforded 11a as a yellow oil (234 mg, 87% yield). Rf= 0.63 (hexanes/EtOAc 90: 10 v/v). MHz, CDCI3) delta 9.42 (br s, 1H), 8.07 (d, .7= 2.3 Hz, 1H), 7.39-7.32 (m, 3H), 7.22 (d, J= 7.8 Hz, 2H), 7.12 (t, J= 8.4 Hz, 2H), 3.91 (s, 3H).13C NMR (101 MHz, CDCI3) delta 168.0, 147.2, 140.3, 136.9, 134.0, 129.6, 124.3, 123.0, 115.9, 113.3, 108.4, 52.2. MS (ESI+) calculated for [Ci4Hi3BrN02]+[M+H]+, 306.0; found 306.1.

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; YALE UNIVERSITY; JORGENSEN, William L.; TRIVEDI-PARMAR, Vinay; (142 pag.)WO2019/178480; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, 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. HPLC of Formula: C7H6INO

General procedure: A two-neck round bottom flask was charged with amagnetic stirrer, evacuated and backfilled with argon. 2-iodobenzamide ( 0.5mmol, 124 mg), aniline or alpha-substituted benzylamine (1.0 mmol), K2CO3(1.0 mmol, 138 mg) and CuBr2 (0.05mmol, 11 mg) in DMSO (5 mL) under argon atmosphere. The mixture was allowed tostir under argon atmosphere at 110 C for 4 h.The mixture was concentrated with the aid of a rotary evaporator, and theresidue was purified by column chromatography on silica gel using petroleumether/ethyl acetate (2:1) as eluent to provide the product 2-9.

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

Reference:
Article; Wang, Li-Xia; Hu, Ben-Quan; Xiang, Jun-Feng; Cui, Jie; Hao, Xiang; Liang, Tong-Ling; Tang, Ya-Lin; Tetrahedron; vol. 70; 45; (2014); p. 8588 – 8591;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-44-8, 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. 626-44-8, name is 1,3,5-Triiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 3 (98.0 mg, 0.211 mmol), 4 (0.06 mL, 0.42 mmol), PdCl2(PPh3)2 (14.8 mg, 0.021 mmol), PPh3 (11.1 mg, 0.042 mmol), CuI (4.0 mg, 0.021 mmol), Et3N (4.0 mL), and THF (5.0 mL) was placed in a round-bottom flask equipped with a magnetic stirring bar. After degassing the reaction mixture several times, the reaction was carried out at 40 ¡ãC for 3 h with stirring. After the reaction mixture was cooled to room temperature, CHCl3 was added to the mixture. The mixture was filtered by Celite, and the solvent was evaporated. The residue was subjected to SiO2 column chromatography (hexane as an eluent) to obtain 6 (30.6 mg, 0.067 mmol, 32percent), S1 (40.2 mg, 0.088 mmol, 42percent), and 5 (4.0 mg, 0.086 mmol, 4percent) as colorless solids.

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, 1,3,5-Triiodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Morisaki, Yasuhiro; Gon, Masayuki; Tsuji, Yuichi; Kajiwara, Yuichi; Chujo, Yoshiki; Tetrahedron Letters; vol. 52; 42; (2011); p. 5504 – 5507;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com