Month: September 2021

619-58-9, name is 4-Iodobenzoic acid, 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. Quality Control of 4-Iodobenzoic acid

i. 4-Iodobenzyl alcohol. To a solution of 4-iodobenzoic acid (22 g) in tetrahydrofuran (450 mL) was added borane dimethylsulfide complex (35.5 mL, 10M in tetrahydrofuran), and the solution was allowed to stir overnight. The reaction was quenched by addition of methanol, and the solvent was evaporated. The residue was dissolved in ethyl acetate and filtered. The solvent was evaporated to give a solid, which was recrystallized from ether to yield a white solid, which was chromatographed, eluding with ether, to give 4-iodobenzyl alcohol (15.1 g).

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

Reference:
Patent; Zeneca Limited; US5521179; (1996); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

608-28-6, Adding a certain compound to certain chemical reactions, such as: 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 608-28-6.

2,2′,6-trimethyl-1,1′-biphenyl (89): To a mixture of Ni-Cat.(0.0125 mmol Nil2+0.025 mmol VIa) and Ar-I 87 (0.036mL, 0.058 g, 0.25 mmol) 1.0 mL of CPME was added. Themixture was stirred for 10 mins. Then the water (0.02 mL,0.02 g, 1.11 mmol) was added. To the mixture, boronic acid88 (0.068 g, 0.5 mmol), bases (0.160 g, 0.75 mmol) wereadded. The reaction mixture was stirred at 105 C. (asmentioned) and aliquot was taken after different time intervalto analyze the data by GC/MS. After that the reactionmixture was filtered through neutral alumina, concentratedunder vacuum, purified by flash chromatography withhexane.1 H NMR (CDC13, 400 MHz): o1.99 (s, 6H), 2.01 (s,3H), 7.05-7.08 (m, lH), 7.14-7.35 (m, 6H); 13C NMR(CDC13, 100 MHz): o19.4, 20.3, 126.0, 126.9, 126.9, 127.2,128.8, 130.0, 135.6, 135.8, 140.5, 141.0.

According to the analysis of related databases, 608-28-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Boehringer Ingelheim International GmbH; Desrosiers, Jean-Nicolas; Fandrick, Daniel Robert; Haddad, Nizar; Li, Guisheng; Patel, Nitinchandra D.; Qu, Bo; Rodriguez, Sonia; Senanayake, Chris Hugh; Sieber, Joshua Daniel; Tan, Zhulin; Wang, Xiao-Jun; Yee, Nathan K.; Zhang, Li; Zhang, Yongda; (58 pag.)US2018/155375; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 672-57-1, 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. 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 5:- Preparation of 7-(2-chloro-5-trifluoromethyl-phenylethynyl)-2-(2,6-dibromo- phenyl)-4,4-dimethyl-l,4-dihydro-chromeno[3,4-d]imidazole:-The mixture of 2-(2,6-dibromo-phenyl)-7-ethynyl-4,4-dimethyl-l,4-dihydro- chromeno[3,4-d]imidazole (0.500 g, 109 mol), dichloro bis (triphenyl phosphine)palladium (II) (0.022 g, 0.0327 mol), tetra butyl ammonium fluoride (0.855 g, 3.27 mol) and l-chloro-2-iodo-4-trifluoromethyl-benzene (0.501 g, 1.63 mol) was heated at 80-90C for 2-3 hours. The reaction mass was quenched in water and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford desired product (0.230 g). ‘HNMR (DMSO- 6): delta 1.65 (s, 6H), 7.09-7.11 (m, 1H), 7.21-7.24 (m, 1H), 7.38-7.44 (m, 1H), 7.52 (m, 1H), 7.77-7.87 (m, 4H), 8.08 (s, 1H), 13.09 (s, 1H).

The synthetic route of 1-Chloro-2-iodo-4-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant Atmaram; GAJERA, Jitendra Maganbhai; NARAYANA, Lakshminarayana; KHAIRATKAR-JOSHI, Neelima; KATTIGE, Vidya Ganapati; WO2012/110860; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 14452-30-3,Some common heterocyclic compound, 14452-30-3, name is 1-(3-Iodophenyl)ethanone, molecular formula is C8H7IO, 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: Arylhalide (1a,b18a,b, 1.2 equiv, typically ca. 50 mg), NNCu(bdmpphen) (1.0 equiv, typically ca. 50 mg), Pd2(dba)3¢CHCl3 (5 mol% in most cases), and DPPF (10 mol% in mostcases) were dissolved in dry THF under nitrogen. The mixturewas refluxed until the starting Cu-complex was consumed(monitored by TLC, typically 30min in most cases for ArI).After the reaction mixture was concentrated under reducedpressure, toluene (3 mL) was added into the residue. The residualmixture was separated and purified by chromatography,to afford the corresponding cross-coupling product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(3-Iodophenyl)ethanone, its application will become more common.

Reference:
Article; Yamada, Kiyomi; Zhang, Xun; Tanimoto, Ryu; Suzuki, Shuichi; Kozaki, Masatoshi; Tanaka, Rika; Okada, Keiji; Bulletin of the Chemical Society of Japan; vol. 91; 7; (2018); p. 1150 – 1157;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 153898-63-6,Some common heterocyclic compound, 153898-63-6, name is 2-Iodo-5-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.

General procedure: a suspension of 3-iodo-4-aminopyridine (1 mmol), methyl 2-mercaptoacetate (1.5 equiv), copper (I) iodide (0.05 mmol), trans-N,N’-dimethylcyclohexane-1,2-diamine (0.1 mmol) and cesium carbonate(2 equiv) in dry 1,4-dioxane (4 mL) in a vial was degassed by bubbling N2 into the suspension for 3 min while stirring. The vial was then capped tightly. The mixture was heated at 100 C (oil bath temperature) for 15 h. After coolingto rt, filtration was carried out. The combined filtrates were concentrated on rotavap and the residue was subjected to silica gel column chromatographpurification (5% methanol in methylene chloride) furnishing 3b as a beige solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-5-methoxyaniline, its application will become more common.

Reference:
Article; Huang, Wei-Sheng; Xu, Rongsong; Dodd, Rory; Shakespeare, William C.; Tetrahedron Letters; vol. 54; 38; (2013); p. 5214 – 5216;,
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. 1450754-38-7, name is 3-(But-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C7H9IN2

(g) Compound 6 (400 mg, 1.6 mmol, 1.0 eq), sodium azide (125 mg, 1.92 mmol, 1.2 eq) and DMF (4 ml) were added to the reaction flask.Raise to 70 C, avoid light reaction for 5 hours; add water to quench,Extract with ethyl acetate, dry, spin dry,A crude product of 200 mg of compound 7,Yield: 76%.

The synthetic route of 1450754-38-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhouguangdian Biological Technology Co., Ltd.; Ni Runyan; Wang Wei; (8 pag.)CN109503615; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 61272-76-2, A common heterocyclic compound, 61272-76-2, name is 4-Fluoro-2-iodoaniline, molecular formula is C6H5FIN, 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: Step B: Pyridine (1.5 mmol) was added to the o-iodo derivative as prepared above (1 mmol) in DCM (5 mL) at 0 °C under nitrogen atmosphere. To this was added methane/p-toluene sulfonyl chloride (1.2 mmol) slowly at 0 °C. Then, the reaction mixture was stirred at room temperature for 5-6 h. After completion of the reaction (monitored by TLC), the reaction mixture was diluted with ethyl acetate (30 mL), washed with 2N HCl solution (10 mL) followed by brine solution (20 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography using ethyl acetate-hexane to give the desired product 2.

The synthetic route of 61272-76-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rambabu; Raja, Guttikonda; Yogi Sreenivas; Seerapu; Lalith Kumar; Deora, Girdhar Singh; Haldar, Devyani; Rao, M.V.Basaveswara; Pal, Manojit; Bioorganic and Medicinal Chemistry Letters; vol. 23; 5; (2013); p. 1351 – 1357;,
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 51839-15-7 as follows. Safety of Dimethyl 5-iodoisophthalate

Dimethyl 5-iodoisophthalate(2.9 g, 8.9 mmol) and THF (50 mL) was cooled to -20 C.,A THF solution (about 14% by mass, 8.4 mL, 8.1 mmol) of isopropyl magnesium chloride-lithium chloride complex was added dropwise.The obtained mixture was stirred at -20 C. for 1 hour,Copper (I) bromide-dimethyl sulfide complex (1.9 g, 9.1 mmol) was added.The resulting mixture was heated to 30 C. and a solution of C60 fullerene (0.72 g, 1.0 mmol) in ODCB (50 mL) was added.The obtained mixture was stirred at 60 C. for 4 hours,Saturated aqueous ammonium chloride solution (1 mL) was added.The resulting mixture was filtered and the volume of the solution was reduced with a rotary evaporator.By adding methanol to the obtained mixture,As a reddish brown solid substance, Compound 7 (C7)(1.5 g, 0.90 mmol,Yield: 90%) was precipitated

According to the analysis of related databases, 51839-15-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Showa Denko; Watanabe, Kentaro; Ueda, Yoshiyuki; Hanawa, Kenzo; (53 pag.)JP2018/203686; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 180624-08-2, 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. 180624-08-2, name is 4-Bromo-2-iodo-6-nitroaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of Intermediate 1A (4.5 g, 13.12 mmol) in EtOH (80 mL) was added concentrated HCl (5.47 mL, 65.6 mmol), followed by tin(II)chloride dihydrate (11.84 g, 52.5 mmol). The reaction mixture was stirred at 60C overnight. After cooled to room temperature, it was treated with an ice-cold 4.0 N NaOH (18 mL) and EtOAc/water. After stirring for 1 min, the white solid was removed by filtration. The filtrate was separated, the organic layer was collected, washed with brine and dried over sodium sulfate. After evaporation of solvent, the crude product was dissolved in a small amount of chloroform and charged to an 80 g silica gel cartridge which was eluted with 5% for 3 min, then a 12 min gradient from 5% to 50%; The desired fractions were combined and concentrated to give Intermediate 1B (3.3 g, 10.55 mmol, 80% yield) as a pale brown solid; 1H NMR (500 MHz, chloroform-d) delta 7.33(d, J=2.2 Hz, 1H), 6.83(d, J=1.9 Hz, 1H), 3.81(br s, 2H), 3.54(br s, 2H); LC-MS: method A, RT=1.82 min; MS (ESI) m/z: 312.8 and 313.8 (M+H)+;

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, 4-Bromo-2-iodo-6-nitroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ZHANG, Xiaojun; ZHENG, Xiaofan; CHUPAK, Louis S.; (102 pag.)WO2017/19828; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 52914-23-5,Some common heterocyclic compound, 52914-23-5, name is 2-(4-Iodophenyl)ethanol, molecular formula is C8H9IO, 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.

Step 1. 2-[(4-Methyl-2-nitroanilino)phenyl]ethanol The title compound was prepared according to the procedure described in step 1 Example 45 from 4-methyl-2-nitroaniline and 4-iodophenylethyl alcohol. 1H-NMR (CDCl3) delta9.35 (1H, br.s), 8.00 (1H, s), 7.33-7.09 (6H, m), 3.91-3.89 (2H, m), 2.89 (2H, t, J=6.4 Hz), 2.30 (3H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(4-Iodophenyl)ethanol, its application will become more common.

Reference:
Patent; Audoly, Laurent; Okumura, Takako; Shimojo, Masato; US2002/77329; (2002); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com