Category: iodides-buliding-blocks

Electric Literature of 31827-94-8, 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows.

Step A18b. A solution of the compound from step A18a (512 mg, 1.86 mmol) in (( (5 mL) was treated with DIPEA (0.45 mL, 2.58 mmol) and MsCl (0.16 mL, 2.07 mmol) for 2 hours at 0 C before being partitioned (CH2Cl2-water). The organics were washed with brine, dried ( a2S04), filtered and evaporated to give the crude desired compound as a colorless oil (725 mg), which was used directly in the next step. ESIMS m/z = 254.20 [M-Boc+2H]+. Step A18c. A solution of the compound from step A18b (1.82 mmol at most) in DMF (5 mL) was treated with 15-crown-5 (80 mg, 0.36 mmol) and al (1.36 g, 9.1 mmol) in the presence of K2CO3 (1.12 g, 8.12 mmol) at 90 C overnight before being cooled down and partitioned (EtO Ac -water). The organics were washed with water, brine, dried ( a2S04), filtered and evaporated. The residue was purified by chromatography (silica, hexanes- ethyl acetate) to give the desired compound as a colorless oil (396 mg, 56%) containing an isomeric impurity. ESIMS m/z = 386.10 [M+H]+. Step A18d. A solution of the compound from step A18c (516 mg, 1.34 mmol) in toluene (10 mL) was treated with totally 4 portions of Bu4SnH (0.36 mL, 1.34 mmol) and AIBN (22 mg, 0.134 mmol) for 12 hours at 110 C before being cooled down and evaporated. The residue was purified by chromatography (silica, hexanes-ethyl acetate) to give the desired compound as a colorless oil (177 mg, 51%) as a single isomer. ESIMS m/z = 260.10 [M+H]+. Step A18e. A solution of the compound from step A18d (170 mg, 0.655 mmol) in CH2CI2 (3 mL) was treated with DAST (0.18 mL, 1.32 mmol) at 0 C for 1 hours before being quenched with aqueous aHC03 dropwisely and partitioned (CH2Cl2-water). The organics were washed with brine, dried ( a2S04), filtered and evaporated. The residue was purified by chromatography (silica, hexanes-ethyl acetate) to give the desired compound as a colorless oil (177 mg, 51%). ESIMS m/z =260.10 [M+H]+. Step A18f. The desired compound was prepared from the compound from step A18e using procedures similar to that described in Intermediate A7. ESIMS m/z = 472.11 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-1-(4-iodophenyl)ethanone. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ENANTA PHARMACEUTICALS, INC.; NOVARTIS AG; QIU, Yao-ling; CAO, Hui; PENG, Xiaowen; GAO, Xuri; OR, Yat, Sun; SWEENEY, Zachary, Kevin; WO2015/17382; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. Safety of 4-Iodo-2-(trifluoromethyl)benzonitrile

[0443] A suspension of trans-1-(4-methoxybenzyl)hexahydropyrano[3,4-d]imidazol-2(3H)-one [racemic (¡À)] (0.25 g, 0.95 mmol), 4-iodo-2-(trifluoromethyl)benzonitrile (0.28 g, 0.95 mmol), trans-N,N?-dimethylcyclohexane-1,2-diamine (0.032 g, 0.29 mmol) and potassium carbonate (0.395 g, 2.86 mmol) in toluene (15 mL) was degassed for 30 min in a microwave vial. CuI (0.009 g, 0.05 mmol) was added and the vial was sealed with an aluminum cap. The sealed vial was kept in a preheated oil bath at 110 C. and stirred for 12 h. The reaction mixture was cooled to RT, filtered through a pad of celite, and filtrates were concentrated under reduced pressure to give a black residue. The residue was purified by column chromatography on silica gel (dichloromethane/methanol=100:0 to 99:1) to give the title compound (0.17 g, 41.0%) as an off white solid. LCMS: m/z 432.1 [M+H]+; 1H NMR (400 MHz, CDCl3) delta 7.80-7.74 (m, 2H), 7.54 (d, 1H), 7.20 (d, 2H), 6.84 (d, 2H), 4.50 (d, 1H), 4.40-4.30 (m, 2H), 4.15-4.05 (m, 1H), 3.80 (s, 3H), 3.65 (ddd, 1H), 3.50-3.20 (m, 2H), 3.10 (ddd, 1H), 1.90 (d, 1H), 1.72-1.68 (m, 1H).

The synthetic route of 4-Iodo-2-(trifluoromethyl)benzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bock, Mark Gary; Chikkanna, Dinesh; Gerspacher, Marc; Khairnar, Vinayak; Lagu, Bharat; Pandit, Chetan; US2014/329858; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 13421-00-6, name is 5-Chloro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 5-Chloro-2-iodobenzoic acid

General procedure: A dry sealable vial was charged with sulfonimidamide 4a (368 mg, 2.00 mmol), 2-iodobenzoic acid (494 mg, 2.00 mmol), CuI (76 mg, 0.40 mmol), and K2CO3 (690 mg, 5.00 mmol) in anhyd DMF (5.0 mL). After heating to 100 C for 2 h, the heterogeneous mixture was cooled to r.t. The mixture was diluted with water (10 mL), acidified with 2 M HCl and extracted with EtOAc (3 ¡Á 30 mL). The combined organic layers were dried (Na2SO4), filtered, and concentrated under reduced pressure. The crude product was purified by CombiFlash chromatography (silica gel, n-hexane/EtOAc, 6:4) to afford the desired product 7a as a cream solid; yield: 633 mg (90%).

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sen, Indira; Sasmal, Swarnendu; Hall, Roger G.; Pal, Sitaram; Synthesis; vol. 48; 21; (2016); p. 3743 – 3752;,
Iodide – Wikipedia,
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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. 69113-59-3, name is 3-Iodobenzonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 3-Iodobenzonitrile

General procedure: Aryl-halide (0.2 mmol, 1 equiv.), Ir(dtbbpy)(ppy)2PF6 (1.8 mg, 0.002 mmol, 1 mol %), NiCl2.glyme (4.4mg, 0.02 mmol, 10 mol %), DMSO (2.0 mL) was added to a 10 mL schlenk flask equipped with a magnetic stirrer bar. This resulting mixture was sealed and degassed via vacuum evacuation and subsequent backfill with ethylene for three times. Then, N,N,N?,N?-tetramethylethylenediamine, TMEDA(60 muL, 2 equiv.), N,N-diisopropylethylamine, DIPEA (70 muL, 2 equiv.) and H2O (7.2 muL, 2 equiv.) were subsequently added in this order. The mixture was then irradiated with blue LED (2 meter strip, 18 W)with ethylene balloon for 24 hours at 80oC (Figure S1). The reaction was added water (30 mL) and extracted with ethyl acetate (10 mL) three times. Combined organic layer was successively washed with brine three times and dried over Na2SO4 and concentrated under reduced pressure. The residue was then subjected to flash column chromatography (hexane or hexane/ethyl acetate) to yield theproduct

The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Jiesheng; Luo, Yixin; Cheo, Han Wen; Lan, Yu; Wu, Jie; Chem; vol. 5; 1; (2019); p. 192 – 203;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, 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. Recommanded Product: 1-Iodo-2-(trifluoromethyl)benzene

General procedure: 9-[2-(4-Nitrophenoxy)naphthalene-1-yl]-11,12-dihydro-10H-indeno[6,5,4-kl]xanthene (3a): A mixture of 1a (73.6 mg, 189 mumol, 1.00 equiv.), 2 (67.1 mg, 198 mumol, 1.05 equiv.), Pd(OAc)2 (4.22 mg, 18.8 mumol, 0.10 equiv.), PPh3 (24.7 mg, 94.0 mumol, 0.50 equiv.) and (nBu)4NOAc (341 mg, 1.13 mmol, 6.00 equiv.) in degassed DMF (5 mL) was stirred at 100 ¡ãC for 21 h. The reaction mixturewas filtered through SiO2, flushed with EtOAc and the solvent of the filtrate was removed in vacuo.Column chromatography (SiO2, n-pentane/EtOAc 20:1) yielded 3

The synthetic route of 1-Iodo-2-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tietze, Lutz F.; Eichhorst, Christoph; Heterocycles; vol. 90; 2; (2015); p. 919 – 927;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 101335-11-9, The chemical industry reduces the impact on the environment during synthesis 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, I believe this compound will play a more active role in future production and life.

Sodium methanethiolate (5g) was added to a solution of 4-fluoro-2-chloro-iodobenzene (18.3g) and stirred for 20h. The mixture was poured into water, extracted with ether, washed with brine, dried (MgS04) and evaporated. Yield 18. 5g. 1H NMR DMSO-d6: 8 7.81 (d, 1H), 7.43 (dd, 1H), 6.98 (dd, 1H), 3.32 (s, 3H)

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, 2-Chloro-4-fluoro-1-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 610-97-9, 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. 610-97-9, name is Methyl 2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Methyl 2-iodobenzoate (25 g, 95 mmol), prop-2-yn-1-ol (8.02 g, 143 mmol) and TEA (26.6 ml, 191 mmol) were added to a deareated mixture of Pd(PPh3)4 (0.220 g, 0.191 mmol), copper(I) iodide (0.073 g, 0.382 mmol) in DMF (60 ml). The resulting mixture was stirred at 90 C. for 5 hrs and then at 40 C. overnight. The reaction mixture was poured into EtOAc (600 ml) and washed with brine (600 ml). Organic phase was then concentrated and the dark oil was rinsed with Et2O (600 ml). The mixture was filtered, and then concentrated to give the title compound as deeply brown oil (13.0 g). This compound was used in the next step without any further purification and characterization. UPLC-MS: 1.53 min, [M+H-18]+. (Method 4)

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

Reference:
Patent; CHIESI FARMACEUTICI S.p.A.; Biagetti, Matteo; Capelli, Anna Maria; Accetta, Alessandro; Carzaniga, Laura; US2015/166549; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 103962-05-6, These common heterocyclic compound, 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, 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 solution of 1-iodo-4-(trifluoromethoxy)benzene (288 mg, 1.0 mmol) and 6-chloro-5-methylpyridin-3-ylboronic acid (223 mg, 1.3 mmol) in DMF (2 mL) was added K2CO3 (552 mg, 4.0 mmol) and H2O (0.5 mL). The reaction mixture was stirred for 5 min under an atmosphere of dry N2. Pd(PPh3)4 (10 mg, 0.009 mmol) was added, and the resulting mixture was subjected to irradiation at 120¡ã C. for 10 min. Cooled, diluted with EtOAc (20 mL), filtered through a layer of celite, washed with 10percent DMF in EtOAc (50 mL), transferred to a separation funnel, organic phase was washed with 2N Na2CO3 (20 mL, 4.00 mmol), H2O (20 mL), 30percent aqueous NH4Cl (50 mL) and brine (50 mL), and dried and concentrated. The crude mixture was subjected to preparative HPLC with a gradient MeCN/H2O (5percent to 98percent) containing 0.1percent TFA to afford 2-chloro-3-methyl-5-(4-(trifluoromethoxy)phenyl)pyridine,MS m/z 288.0 (M+H), HPLC purity>97percent.

The synthetic route of 103962-05-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Gilead Palo Alto, Inc.; US2011/21521; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 88-67-5, name is 2-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. Application In Synthesis of 2-Iodobenzoic acid

2.48 g (10 mmol) of o-iodobenzoic acid was weighed, and 5 mL of absolute ethanol was weighed. Magnetic seeds were placed in a round bottom flask, and an appropriate amount of concentrated sulfuric acid was added thereto, and the mixture was stirred at 90 C for 12 hours, and detected by TLC, and stopped when the raw materials disappeared. reaction. The reaction solution was concentrated by a reduced pressure rotary evaporator to remove excess ethanol, and an appropriate amount of saturated NaHCO 3 was added to neutralize the remaining concentrated sulfuric acid.When no bubbles are generated, that is, when the neutralization is complete, the mixture is washed with ethyl acetate (3¡Á50 mL) and water, and the organic layer is combined, water is evaporated, and filtered, and then filtered, and then filtered, and then evaporated. The ethyl acetate was removed to give 2.50 g of ethyl iodobenzoate as a yellow oil, yield 90%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 88-67-5, its application will become more common.

Reference:
Patent; Xinxiang Medical University; Xinxiang Medical School San Quan College; Yan Fulin; Wang Yawen; Yan Jianwei; Yin Tiantian; Ma Jinshuo; (15 pag.)CN110183387; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 54413-93-3, The chemical industry reduces the impact on the environment during synthesis 54413-93-3, name is 2-Iodo-5-methoxybenzoic acid, I believe this compound will play a more active role in future production and life.

General procedure: In a 10 mL glass tube 2-iodobenzoic acid (1.0 mmol), acetamidine hydrochloride (1.2 mmol), CuCl2 (0.1 mmol), L2 (0.1 mmol), and NaOH (4.0 equiv.) and 3.0 mL water were placed. The vessel was then sealed with a septum and placed into the microwave cavity. Initial microwave irradiation of 120 W by using a CEM Discover microwave synthesizer was used at the room temperature for 20 min. The reaction mixture was stirred continuously during the reaction. After completion of the reaction, the solvent was removed in vacuo. The residue was purified by silica gel column chromatography to afford the corresponding product. All the products were confirmed by NMR and MS spectroscopic analysis.

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, 2-Iodo-5-methoxybenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ke, Fang; Liu, Caiqin; Zhang, Peng; Xu, Jianhua; Chen, Xiaole; Synthetic Communications; vol. 48; 24; (2018); p. 3089 – 3098;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com