Tag: M.W=200-300

Electric Literature of 6293-83-0,Some common heterocyclic compound, 6293-83-0, name is 2-Iodo-4-nitroaniline, molecular formula is C6H5IN2O2, 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.

EXAMPLE 11 Preparation of 2-Iodo-p-phenylenediamine A mixture of concentrated hydrochloric acid (150 ml) and 2-iodo-4-nitroaniline (30.0 g) is stirred and warmed to 45¡ã-50¡ã C. A solution of stannous chloride dihydrate (90.0 g) in concentrated hydrochloric acid (110 ml) is added while maintaining the reaction temperature at 65¡ã-70¡ã C. After the addition is completed, the mixture is cooled in an ice bath and 50percent sodium hydroxide (250 ml) is added slowly. The mixture is filtered and the isolated damp solid is stirred in 600 ml water at reflux. The solution is decolorized with charcoal, filtered and cooled to afford 5.55 g of title compound, m.p. 95¡ã-99¡ã C.

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-4-nitroaniline, its application will become more common.

Reference:
Patent; American Cyanamid Company; US4239708; (1980); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 54413-93-3, These common heterocyclic compound, 54413-93-3, name is 2-Iodo-5-methoxybenzoic 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.

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.

The synthetic route of 54413-93-3 has been constantly updated, and we look forward to future research findings.

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

Adding a certain compound to certain chemical reactions, such as: 105202-02-6, name is 2-Iodo-5-(trifluoromethyl)aniline, 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 105202-02-6, Product Details of 105202-02-6

To a solution of compound 53 (620 mg, 2.16 mmol) in DMF (5 mL) was added phenylacetylene (331 mg, 356 muL, 3.24 mmol), PdCI2(PPh3)2 (76 mg, 0.108 mmol), Cul (25 mg, 0.131 mmol) and Et3N (656 mg, 903 muL, 6.48 mmol) at 23 C. The reaction mixture was stirred for 6 h at 23 C before it was quenched with a saturated solution of NH4CI (10 mL) and diluted with EtOAc (50 mL). The layers were separated, and the organic layer was extracted with H20 (3 x 10 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexanes:EtOAc 5: 1 ) to give compound 54 (518 mg, 92%) as pale yellow solid. (0472) [00362] 1 H NMR (400 MHz, CDCI3) delta = 7.56 (m, 2H), 7.47 (dd, J = 8.5, 0.8 Hz, 1 H), 7.42 – 7.38 (m, 3H), 6.98 – 6.96 (m, 2H), 4.48 (brs, 2H); 13C NMR (101 MHz, CDCI3) delta = 147.8, 132.5, 131 .6, 131 .5 (q, J = 32.2 Hz), 128.7, 128.5, 124.0 (q, J = 272.3 Hz), 122.6, 1 14.3 (q, J = 3.8 Hz), 1 1 1 .2, 1 10.7 (q, J = 4.0 Hz), 96.5, 84.6; 19F NMR (376 MHz, CDCI3) delta = -63.13. m/z (ESI) 262.1 [M+H+].

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:
Patent; THE GOVERNING COUNCIL OF THE UNIVERSITY OF TORONTO; GREIG, Iain; ZANDA, Matteo; TSENG, Chih-Chung; ROSS, Ruth; (134 pag.)WO2016/29310; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 6940-76-7, These common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, 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.

Sodium hydride (1.96 g, 49.337 mmol, 60% suspension in mineral oil) was treated with DMF (60 mL), followed by 6-nitroindole (6) (2.0 g, 12.334 mmol) in DMF (20 mL) over a period of 5 min at 0 C. After stirring for 15 min, the solution was treated with 1-chloro-3-iodopropane (3.9 mL, 37.002 mmol), the reaction was brought to room temperature and stirred for 3 h. The reaction was quenched with saturated brine (80 mL), water (80 mL) and cooled to 0 C. The solid was filtered off, washed with water (50-75 mL) and dried to obtain the crude product. The crude product was recrystallised from hot toluene (10 mL)/hexanes (5 mL) to obtain compound 148 (2.637 g, 90%) as solid. mp 85-87 C.; 1H-NMR (CDCl3) delta 2.28-2.36 (m, 2H), 3.46 (t, 2H, J=5.7 Hz), 4.45 (t, 2H, J=6.6 Hz), 6.62 (d, 1H, J=2.7 Hz), 7.43 (d, 1H, J=3.0 Hz), 7.66 (d, 1H, J=8.7 Hz), 8.02 (dd, 1H, J=1.8, 7.9 Hz), 8.36 (d, 1H, J=0.9 Hz).

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Maddaford, Shawn; Ramnauth, Jailall; Rakhit, Suman; Patman, Joanne; Renton, Paul; Annedi, Subhash C.; US2006/258721; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 25245-35-6, name is 2-Iodo-1,4-dimethoxybenzene, 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 25245-35-6, SDS of cas: 25245-35-6

To a stirred solution of 2-iodo-1,4-dimethoxybenzene (4b, 264 mg; 1.0 mmol) and tert-butyl alcohol (0.25 mL) in glacialacetic acid (0.2 mL) at 0 C was added dropwise over 2 min concentrated H2SO4 (0.3mL). The reaction was stirred at 0 C for 2 h and then allowed to warm to roomtemperature and stirred overnight. Work up consisted of partitioning the reaction mixturebetween water and ethyl acetate, followed by washing the organic layer with dil. aqNaHCO3, water and drying (Na2SO4). Preparative TLC (hexane-CH2Cl2, 1:1) producedrecovered starting material (67 mg) and the product (148 mg; 46%; 62% based onrecovered starting material). Mp 79-82 C (Lit: 81-83 C [3]). 1H-NMR (CDCl3, 500MHz): 1.35 (s, 9H, But), 3.79 (s, 3H, OCH3), 3.83 (s, 3H, OCH3), 6.81 (s, 1H), 7.20 (s,1H).

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-1,4-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kempton, Robert J.; Kidd-Kautz, Taylor A.; Laurenceau, Soizic; Paula, Stefan; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 971 – 975;,
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. 3718-88-5, name is 3-Iodobenzylamine hydrochloride, A new synthetic method of this compound is introduced below., Computed Properties of C7H9ClIN

take 5.88 g (21.8 mmol) 3-iodobenzylamine hydrochloride (C1) and 2.06 g (47.96 mmol) cyanamide (C2) to form a mixture that is heated and refluxed at 105 degrees Celsius for 4 hours. After cooling down, add water (10 mL) into the mixture to dissolve completely. Then add 10 mL aqueous solution of sodium bicarbonate (C3) (1.83 g, 21.8 mmol) to obtain an insoluble solid (precipitate). After filtering, washing with cold water, acetone and ether and drying, the compound C4 (6.7 g, 91%) is obtained.Analysis of the synthesis product: IR (KBr) nu 3352 (NH), 1697 (CO) cm-1. 1H NMR (CD3OD) delta 7.71 (s, 1 H, C6H4), 7.68 (d, J=7.8 Hz, 1 H, C6H4), 7.33 (d, J=7.8 Hz, 1 H, C6H4), 7.15 (t, J=7.8 Hz, 1 H, C6H4), 4.36 (s, 2 H, CH2). 13C NMR (CD3OD) delta 160.51 (CO), 157.67 (CN), 139.27, 136.92, 136.12, 130.52, 126.41 and 94.0 (C6H4), 43.58 (CH2)

The synthetic route of 3718-88-5 has been constantly updated, and we look forward to future research findings.

Electric Literature of 52548-14-8, 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. 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

Part A. 2-iodo-5-methyl-benzoic acid benzyl ester A solution of 2-iodo-5-methylbenzoic acid (2 g, 7.6 mmol) in 20 ml DMF was treated with KHCO3 (0.92 g, 9.2 mmol) and then benzyl bromide (1.1 mL, 9.2 mmol). The resulting mixture was stirred overnight at rt under N2. Reaction was poured into water and extracted 3* with EtOAc. Combined extracts were washed with sat’d. NaHCO3 and brine, dried over anh.Na2SO4, filtered and evaporated. Flash chromatography gave the pure benzyl ester (2.62 g, 98%) as a colorless liquid.

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

Application of 111771-08-5, 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. 111771-08-5, name is 2-Fluoro-6-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step A: (Z)-N’-((2-Fluoro-6-iodobenzoyl)oxy)acetimidamide. To a heterogeneous mixture of 2-fluoro-6-iodobenzoic acid (1 .51 g, 5.66 mmol) at 0 C in DCM (28 mL) was added oxalyl chloride (0.635 mL, 7.36 mmol) followed by DMF (0.15 mL). Gas evolution commenced immediately and after 5 min the ice bath was removed. When gas evolution had ceased and the mixture was homogeneous an aliquot was removed and quenched with MeOH. Formation of the methyl ester was confirmed by HPLC and the mixture was concentrated in vacuo. The viscous liquid was dissolved in fresh DCM (28 mL) and treated with solid N-hydroxyacetamidine (503 mg, 6.79 mmol) in several portions followed by TEA (1 .2 mL, 8.49 mmol) at 0 C. After stirring for 14 h at ambient temperature the mixture was washed with saturated aqueous NaHCO3 solution. The combined organic extracts were dried over Na2SO4, filtered andconcentrated in vacuo. Chromatography (Hex to 100% EtOAc/Hex) afforded the desired product as a colorless oil (1 .57 g, 86%). MS (ESI) mass calculated for C9H8FIN2O2, 321 .96; m/z found, 323.0. 1 H NMR (500 MHz, CDCI3): 7.70 – 7.65 (m, 1 H), 7.15 – 7.1 1 (m, 2H), 4.87 (br s, 2H), 2.06 (s, 3H).

The synthetic route of 2-Fluoro-6-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Electric Literature of 2468-56-6,Some common heterocyclic compound, 2468-56-6, name is 6-Iodohex-1-yne, molecular formula is C6H9I, 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: Concentrated sulfuric acid (0.15 mL) was added under stirring at ambient temperature to a suspension of 25 mmole of uracil 3 or uracil derivatives, namely 6-methyluracil 4, thymine 5, quinazoline-2,4(1H,3H)-dione 6 and hexamethyldisilazane (HMDS, 62.5 mmol) in 100 mL of toluene. The mixture was refluxed for 4 h, the solvent and excessive HMDS were removed to afford bis(trimethylsilyl) ether derivative 7. This crude product was engaged in the next step without any previous purification. A solution of 40 mmole of appropriate alkyne (propargyl bromide, 5-iodo-1-pentyne, 6-iodo-1-hexyne) in DMF (3 mL) was added to the crude product 7 and the reaction mixture was stirred at 115-130 C for 12 h. After the solvent was distilled off under reduced pressure, 200 ml of chloroform was added to the residue, and the mixture was filtered. The filtrate was concentrated, and the residue was purified by column chromatography on silica gel using as eluent first petroleum ether, then petroleum ether-ethyl acetate (1.5:1) and then ethyl acetate. From the third fraction the target N1-alkynyl-3,4-dihydro-2,4-dioxopyrimidines (3a,b, 4b,c, 5a,b, 6a,b) were isolated.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6-Iodohex-1-yne, its application will become more common.

Application of 191348-14-8, 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. 191348-14-8, name is 2-Iodo-4-methoxyaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under anhydrous and anaerobic conditions, 0.1 mmol of 2-iodo-4-methoxyaniline was added.0.12 mmol of 2-trifluoromethyl 4-methoxybenzaldehyde, 0.3 mmol of selenium powder, 0.005 mmol of copper, 0.2 mmol of potassium hydroxide and 10 ml of DMSO solution,The reaction was refluxed at 120 C in a single-neck round bottom flask, and the reaction was monitored by TLC.Separation of pure methoxy-containing benzoselenazole compounds by column chromatographyThe reaction product was obtained by demethylation of boron tribromide (6 eq.).The product is a pale yellow oily compound.The yield was 25%.

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