Tag: M.W=200-300

Related Products of 460-37-7, 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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Example 302A Ethyl [6-formyl-5-methyl-2,4-dioxo-1-(3,3,3-trifluoropropyl)-1,4-dihydrothieno[2,3-d]pyrimidin-3(2H)-yl]acetate 1.0 g (3.37 mmol) of the compound from Ex. 289A and 1.65 g (5.06 mmol) of caesium carbonate were stirred in 17 ml of DMF at RT for 10 min, before 1.13 g (5.06 mmol) of 1,1,1-trifluoro-3-iodopropane were added. Subsequently, the reaction mixture was stirred at a temperature of 100 C. in a microwave oven (Biotage Initiator with dynamic control of irradiation power). After 1.5 h, the mixture was cooled to RT, diluted with about 75 ml of ethyl acetate and washed successively with water and saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the filtrate was evaporated to dryness. The crude product was purified by preparative HPLC (Method 8). After concentration of the product fractions and drying under high vacuum, 938 g (70% of theory) of the title compound were obtained. 1H-NMR (500 MHz, DMSO-d6, delta/ppm): 10.12 (s, 1H), 4.64 (s, 2H), 4.22 (t, 2H), 4.15 (q, 2H), 2.89-2.74 (m, 2H), 2.79 (s, 3H), 1.21 (t, 3H). LC/MS (Method 1, ESIpos): Rt=0.98 min, m/z=393 [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, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
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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,
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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,
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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,
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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

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

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 167479-01-8 as follows. COA of Formula: C8H16INO2

(25) Synthesis of methyl 1-(3-tert-butoxycarbonylaminopropyl)-2-indolecarboxylate: The reaction was carried out in a manner similar to Reference Example 5 except for using 5.00 g (28.5 mmol) of methyl 2-indolecarboxylate, 1.26 g (31.4 mmol) of 60% sodium hydroxide, 12.3 g (43.2 mmol) of tert-butyl N-(3-iodopropyl)carbamate (prepared from 3-iodopropyl-amine and di-tert-butyl dicarbonate) and 60 ml of dimethylformamide. Thus, 2.54 g (27%) of methyl 1-(3-tert-butoxycarbonylaminopropyl)-2-indolecarboxylate was obtained. 1H NMR (CDCl3) delta: 1.45 (9H, 8), 1.90-2.10 (2H, m), 3.00-3.20 (2H, m), 3.91 (3H, s), 4.62 (2H, t, J=6.9 Hz), 4.98 (1H, br-s), 7.06-7.20 (1H, m), 7.28-7.44 (3H, m), 7.68 (1H, d, J=7.3 Hz).

According to the analysis of related databases, 167479-01-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Sumitomo Pharmaceutical Co., Ltd.; US6169107; (2001); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, 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 5876-51-7, name: 5-Iodobenzo[d][1,3]dioxole

To a solution of tetrabutylammonium bromide (1.100 g, 3.33 mmol), potassium acetate (0.586 g, 3.57 mmol), palladium acetate (0.025 g, 0.11 mmol) in DMF (20 mL) were added 3,4-methylenedioxy-iodobenzene (2.21 mmol) and 4-ethenylpyridine (2.44 mmol). The reaction mixture was recharged with Argon and stirred at 80C for 5 h in a sealed tube. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl and concentrated in vacuo. The residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 10:3) to afford the desired product (E)-4-(2-(benzo[d][1,3]dioxol-5-yl)vinyl)pyridine (71) (Yield 37.5%, Purity 96.2%, CAS: 651741-80-9) as a yellow amorphous solid.HRMS (ESI) (M+H)+m/z226.0861, calcd for C14H12NO2226.0863.1H NMR (CDCl3, 500 MHz) delta: 8.51 (d,J= 5.0 Hz, 2H), 7.22 (d,J= 5.5 Hz, 2H), 7.11 (d,J= 16.5 Hz, 1H), 7.00 (s, 1H), 6.90 (d,J= 8.0 Hz, 1H), 6.72-6.76 (m, 2H), 5.91 (s, 2H).13C NMR (CDCl3, 125 MHz) delta: 149.7, 147.9, 147.9, 144.3, 132.3, 130.2, 123.7, 122.1, 120.2, 108.1, 105.4, 101.0.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Liang, Jian-Hua; Yang, Liang; Wu, Si; Liu, Si-Si; Cushman, Mark; Tian, Jing; Li, Nuo-Min; Yang, Qing-Hu; Zhang, He-Ao; Qiu, Yun-Jie; Xiang, Lin; Ma, Cong-Xuan; Li, Xue-Meng; Qing, Hong; European Journal of Medicinal Chemistry; vol. 136; (2017); p. 382 – 392;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 128140-82-9, 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. 128140-82-9, name is 1-(Difluoromethoxy)-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Step a) 1-(Difluoromethoxy)-4-(phenylethynyl)benzene Into a mixture of ethynylbenzene (1.9 g, 18.5 mmol), 1-(difluoromethoxy)-4-iodobenzene (5 g, 18.5 mmol), N,N-dimethylformamide (35 mL), and triethylamine (12.8 mL, 92.6 mmol) was introduced anhydrous argon for 5 minutes. Then, copper(I) iodide (1.85 mmol, 351 mg) and dichlorobis(triphenylphosphine)palladium(II) (1.11, 0.71 g) were added into the mixture and the new mixture was stirred at 60 C. for 3 hours. The mixture cooled to room temperature, poured into water and extracted with ethyl ether. The organic extracts were dried over MgSO4. Evaporation and purification on silica gel (ISCO) using hexanes/EtOAc (100/1) as the eluding solvent, gave 1-(difluoromethoxy)-4-(phenylethynyl)benzene as a clear oil (3.45 g, 76% yield). MS m/e M+ 244; 1H NMR (400 MHz, DMSO-d6) delta 7.2 (d, J=8.78 Hz, 2H), 7.28-7.45 (m, 4H), 7.5-7.55 (m, 2H), 7.6 (d, J=7.78 Hz, 2H).

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

Reference:
Patent; Wyeth; US2007/72925; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 16932-44-8,Some common heterocyclic compound, 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, molecular formula is C8H9IO2, 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: An argon-filled flask wasadd the respective aryl halide (1.0 mmol), CuI (20 mg, 0.1 mmol, 10 mol%), L3(37 mg, 0.1 mmol, 10 mol%), KOH (168 mg, 3 mmol), thiol (1.5 mmol) and glycerol(10 mL). The contents were then stirred at 100 C for 24 h. After that, themixture was cool to room temperature, diluted with ethyl acetate (20 mL) and washedwith saturated NaCl solution (3 x 20 mL). The organic layer was separated,dried over MgSO4 and concentrated under vacuum. The crude productwas purified by flash chromatography on silica gel using hexane /ethyl acetateas eluent

The synthetic route of 16932-44-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Cargnelutti, Roberta; Lang, Ernesto S.; Schumacher, Ricardo F.; Tetrahedron Letters; vol. 56; 37; (2015); p. 5218 – 5222;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com