Tag: M.W=200-300

Electric Literature of 19230-28-5, 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. 19230-28-5, name is 1,3-Dichloro-2-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of 1,3-dimethyluracil 1a (0.20 mmol) in 2,2,2-trifluoroethanol (TFE) (3 mL), (4-chlorophenyl)(hydroxy)iodonium tosylate 2f (0.22 mmol) was added and it was stirred at room temperature. After completion of the reaction, the solvent was removed under vacuum. The product was then precipitated by the addition of Et2O with stirring. The precipitate was filtered to give uracil-iodonium(III) salt 3af-OTs as a white powder.

The chemical industry reduces the impact on the environment during synthesis 1,3-Dichloro-2-iodobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Takenaga, Naoko; Hayashi, Takumi; Ueda, Shohei; Satake, Hiroyuki; Yamada, Yoichi; Kodama, Tetsuya; Dohi, Toshifumi; Molecules; vol. 24; 17; (2019);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 59382-39-7, name is 1-Fluoro-4-iodo-2-(trifluoromethyl)benzene, 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 59382-39-7, Formula: C7H3F4I

(69-1) Synthesis of 3-(4-fluoro-3-trifluoromethylphenyl)-2-propyne-1-ol (compound 69-1) A mixture of 2-fluoro-5-iodobenzotrifluoride (5.00 g), copper(I) iodide (65.5 mg), triphenylphosphine (226 mg), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (356 mg), propargyl alcohol (1.12 ml), diisopropylethylamine (12.0 ml) and tetrahydrofuran (80 ml) was stirred at room temperature for 11 hr. The reaction mixture was added to brine, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1 – 80:20) to give the object product (3.26 g) as a brown oil. 1H-NMR(CDCl3) delta (ppm): 1.69(1H, t, J=6.2Hz), 4.50(2H, d, J=6.2Hz), 7.16(1H, t, J=9.3Hz), 7.58-7.62(1H, m), 7.69(1H, dd, J=1.4, 6.8Hz).

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-Fluoro-4-iodo-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; EP2168944; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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. 19094-56-5

General procedure: To a stirred suspension of 2-chloro-5-iodobenzoic acid(5.65 g, 0.02 mol) in CH2Cl2(20 mL) was added oxalylchloride(1.80 mL, 0.021 mol) and DMF(0.02 mL). Theresulting mixture was stirred for 4 h at room temperature.The mixture was concentrated, and the residual colorlesssolid was dissolved in CH2Cl2(40 mL). To this solutionwere added corresponding substituted benzene(0.02 mol)and then AlCl3(2.75 g, 0.021 mol) portionwise so that thetemperature did not exceed 0 C. After being stirred at 10-20 C for 3 h, the mixture was poured into ice water andextracted with CH2Cl2 three times. The combined organiclayers were washed with 1M HCl, water, and brine, thendried over MgSO4 and concentrated. The residual solid wascrystallized from ethanol to give as white solid.According to this procedure the following compoundswere prepared.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 19094-56-5.

Reference:
Article; Hu, Shengquan; Sun, Wuji; Wang, Yeming; Yan, Hong; Medicinal Chemistry Research; vol. 28; 4; (2019); p. 465 – 472;,
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. 612-55-5, name is 2-Iodonaphthalene, A new synthetic method of this compound is introduced below., name: 2-Iodonaphthalene

General procedure: A mixture of aryl halide (1.0 mmol), alkene (1.1 mmol), triethylamine (2 mmol), DMF (5 mL), and the catalyst (30 mg, 0.28 mol% Pd ) was stirred at 80 C for an appropriate time under aerial condition. The progress of the reaction was monitored by TLC. After completion of the reaction, the mixture was cooled to room temperature, poured into H2O (10 mL), and the catalyst was separated by magnetic decantation. In the case of acrylic acid, aqueous solution of Na2CO3 (10 mL, 3% w/v) was added; after separation of the catalyst, and the product was extracted with ethyl acetate (3 × 10 mL). The combined organic extracts were washed with brine (2 × 10 mL), dried over MgSO4, and concentrated in vacuum. The crude product was further purified by column chromatography (silica mesh size 60-120).

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; Vibhute, Sandip P.; Mhaldar, Pradeep M.; Shejwal, Rajendra V.; Rashinkar, Gajanan S.; Pore, Dattaprasad M.; Tetrahedron Letters; vol. 61; 17; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 54413-93-3,Some common heterocyclic compound, 54413-93-3, name is 2-Iodo-5-methoxybenzoic acid, molecular formula is C8H7IO3, 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 stirred solution of 2-iodobenzoic acids a (10 mmol) in CH2Cl2, was added DCC (dicyclohexylcarbodiimide, 11 mmol), DMAP (Dimethylaminopyridine, 2 mmol) and alcohols b (10 mmol) in sequence. The resulting solution was stirred overnight at room temperature then filtered through a sand core funnel and washed with diethyl ether (2 x 40mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to obtain the pure product c in moderate to good yields. To a soluton of 2-iodobenzoates c in Et3N (5 mL) was added PdCl2 (PPh3)2 (4 mol percent) and CuI (2 mol percent) and the reaction vial was flushed with Ar and the reaction mixture was stirred for 5 minutes. A solution of propargyl alcohols d (1.05 equiv) in Et3N (5 mL) were then added dropwise through a syringe for 5 minutes. The resulting solution was stirred at room temperature overnight. When the reaction was considered complete as determined by TLC analysis, the mixture was quenched by addition of saturated aqueous ammonium chloride (10 mL) and extracted with ethyl ether (3 x 40 mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to give 1.

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-methoxybenzoic acid, its application will become more common.

Reference:
Article; Zhu, Hai-Tao; Tong, Xiao-Juan; Zhou, Ni-Ni; Yang, De-Suo; Fan, Ming-Jin; Tetrahedron Letters; vol. 57; 49; (2016); p. 5497 – 5500;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 5458-84-4,Some common heterocyclic compound, 5458-84-4, name is 1-Iodo-2-methoxy-4-nitrobenzene, molecular formula is C7H6INO3, 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.

Add 1.0 g (3.58 mmol) of 1-iodo-2-methoxy-4-nitrobenzene to a 50 ml two-port bottle and turn on magnetic stirring.Add 15 ml of 95% ethanol at room temperature.Stir for 30min;Adding an appropriate amount of zinc particles to dilute hydrochloric acid for activation;0.8 (12 mmol) of activated zinc particles were sequentially added to the double-mouth bottle.10ml of 20% hydrochloric acid solution,Stirring at room temperature for 72 h;After the reaction,Stop the reaction,The obtained reaction solution was extracted with ethyl acetate.After salt washing, remove the water layer.After the obtained organic phase is distilled under reduced pressure,The dark red solid product, 2-methoxy-4-iodoaniline, 2.18 g was obtained in a yield of 81.23%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Iodo-2-methoxy-4-nitrobenzene, its application will become more common.

Reference:
Patent; Ningxia University; Yang Jinhui; Chi Jiurong; Yan Zhiming; Feng Yueji; Wang Shihaozhi; (5 pag.)CN109776331; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 167479-01-8, 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. 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of an aminoalcohol (66.6 mmol) in THF (67 mL) was added di-tert-butyl dicarbonate (15.3 g, 66.6 mmol) at 50 C under an argon atmosphere. After 3 h stirring, the solvent was removed in vacuo. The crude product was purified by silica gel column chromatography (EtOAc / hexane, 50:50) to give a N-Boc aminoalcohol. Iodine (12.5 g, 49.3 mmol) was added to a solution of N-Boc aminoalcohol (17.6 mmol), PPh3 (6.92 g, 26.3 mmol) and imidazole (1.79 g, 26.3 mmol) in CH2Cl2 (98 mL) at 0 C. The mixture was stirred at room temperature for 1 h under an argon atmosphere. The reaction mixture was quenched with saturated aqueous Na2S2O3, diluted with CH2Cl2 and extracted with CH2Cl2. The organic layer was washed with H2O and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane, 10:90) to afford a N-BOC aminoalkyliodide. To a solution of NaH (60% in oil, 0.673 g, 16.8 mmol) in DMF (15.3 mL) was added dropwise a solution of N-hydroxyphthalimide (2.49 mmol) in DMF (10 mL) at 0 C under an argon atmosphere. After 15 min of stirring, a solution of the iodide (15.3 mmol) in DMF (10 mL) was added dropwise to the solution and stirred at 70 C for 12 h. After cooled to 0 C, the reaction was quenched with H2O and filtrated to afford colorless solid, which was recrystallized to give a N-alkoxyphthalimide 13a-d.

The synthetic route of tert-Butyl (3-iodopropyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fukuda, Hiroshi; Nishikawa, Keisuke; Fukunaga, Yukihiro; Okuda, Katsuhiro; Kodama, Kozue; Matsumoto, Kenji; Kano, Arihiro; Shindo, Mitsuru; Tetrahedron; vol. 72; 41; (2016); p. 6492 – 6498;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, 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 1,2-Dichloro-3-iodobenzene

EXAMPLE 25A [(2,3-dichlorophenyl)ethynyl](trimethyl)silane 1,2-Dichloro-3-iodobenzene (4.95 g, 18.1 mmol), trimethylsilylacetylene (2 g, 20 mmol), bis(triphenylphosphine)palladium(II)chloride (245 mg, 0.35 mmol), and copper(I)iodide (45 mg, 0.24 mmol) were combined in triethylamine (120 mL) and heated at reflux for 45 minutes. The mixture was allowed to cool to room temperature and was then partitioned between diethyl ether and saturated sodium chloride. The organic phase was dried with sodium sulfate, filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was taken directly on to the next step.

The synthetic route of 1,2-Dichloro-3-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Carroll, William A.; Florjancic, Alan S.; Perez-Medrano, Arturo; Peddi, Sridhar; US2007/105842; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 351003-36-6, 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. 351003-36-6 name is 2-Fluoro-5-iodobenzonitrile, 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.

Step 2: 3-(3-Cvano-4-fluorophenyl)-N-(2,4-dimethoxybenzyl)prop-2-yti-l-aminium chloride (F2)To a solution of lambda/-(2,4-dimethoxybenzyl)prop-2-yn-l -amine (1 eq) in a mixture of DMF and Et3N (4:1) was added 2-fiuoro-5-iodobenzonitrile (1.5 eq), CuI (0.2 eq) and Pd(PPh3)4 (0.1 eq). The resulting mixture was stirred at RT overnight. The reaction mixture was diluted with EtOAc, washed with 0.1 N HCl (2x) and then with brine; dried (Na2SO4), filtered and concentrated under reduced pressure. Treatment with an excess of 2N HCl solution in Et2O provided the desired compound after concentration under reduced pressure.1H NMR (400 MHz, DMSOd6) delta: 9.55 (2H, br. S), 8.12 (IH, dd, J = 5.9, 1.6 Hz), 7.96-7.85 (IH, m), 7.62 (IH, t, J = 9.0 Hz), 7.39 (IH, d, J = 8.3 Hz), 6.63 (IH, d, J = 1.8 Hz), 6.58 (IH, dd, J = 8.3, 1.8 Hz), 4.17 (2H, s), 4.09 (2H, s), 3.82 (3H, s), 3.78 (3H, s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Fluoro-5-iodobenzonitrile, and friends who are interested can also refer to it.

Reference:
Patent; ISTITUTO DI RICERCHE DI BIOLOGIA MOLECOLARE P. ANGELETTI SPA; WO2007/138355; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 33348-34-4, name is 4-Amino-3-iodobenzonitrile, 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 33348-34-4, Quality Control of 4-Amino-3-iodobenzonitrile

General procedure: An oven-dried flask was charged with o-iodoaniline (13 mmol), the corresponding benzyl bromide(10 mmol), NaHCO3 (20 mmol), and DMF (20 mL). The mixture was stirred at 50 C under air for 3-4 h.After the completion of the reaction (monitored by TLC), the reaction mixture was cooled to ambienttemperature and 15 mL water was added to the mixture, then extracted by EtOAc for 3 times (3 × 30 mL).The combined extracts were washed with brine, dried over Na2SO4, and the solvent was removed in vacuoto provide a crude product, which was purified by column chromatography on silica gel to afford pure product.

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-Amino-3-iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chen, Zhengkai; Li, Hongli; Cao, Gangjian; Xu, Jianfeng; Miao, Maozhong; Ren, Hongjun; Synlett; vol. 28; 4; (2017); p. 504 – 508;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com