Category: 60-56-0

Related Products of 60-56-0,Some common heterocyclic compound, 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, molecular formula is C4H6N2S, 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 mixing of thiols (1 mmol), sodium hydroxide(1.1 mmol), water (0.5 mL) and methanol (3 mL) were stirred in room temperature. After 30 min,compound 2 (1.1 mmol) in 5 mL CH2Cl2 was added dropwise to the mixture for 36 h-42 h. The mixturewas concentrated in vacuo. The residue was dissolved by CH2Cl2. The solution was extracted threetimes with water. The organic phase was dried overnight with anhydrous sodium sulfate. The solventwas concentrated in vacuo to give crude products. The crude product was purified by silica gelcolumn chromatography.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Methyl-1H-imidazole-2(3H)-thione, its application will become more common.

Reference:
Article; Yi, Yunpeng; Fu, Yunxing; Dong, Pengcheng; Qin, Wenwen; Liu, Yu; Liang, Jiangping; Shang, Ruofeng; Molecules; vol. 22; 6; (2017);,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Adding a certain compound to certain chemical reactions, such as: 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, belongs to imidazoles-derivatives 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 60-56-0, SDS of cas: 60-56-0

2-mercapto-1-methylimidazole (400 mg, 3.5 mmol) was mixed with K2CO3 (968 mg, 7 mmol) in N, N-dimethylformamide (N, N-dimethylformamide ) (7 mL), followed by addition of di-tert-butyl dicarbonate (1.1 mL, 5.2 mmol). The resulting mixture was then stirred at 60 C for 30 minutes in a nitrogen atmosphere, followed by partitioning with ethyl acetate (40 mL) and water (20 mL). The ethyl acetate layer was then collected and washed with brine (brine), dried over anhydrous MgSO4, and then concentrated under vacuum. Thereafter, the resulting residue was purified by silica gel column chromatography to give a compound (665 mg, yield 89%) as a pale yellow solid.

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; HUNGKUANG UNIVERSITY; Chan, JinFeng; Chen, MingRen; LAI, SHITING; GUO, YIQIN; (36 pag.)TW2016/7932; (2016); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

These common heterocyclic compound, 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, 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. Product Details of 60-56-0

EXAMPLE 4 1-methyl-2-[3-[(p-isobutyloxycarbonyl)-phenoxy]-2-hydroxy-propylthio]-imidazole hydrochloride The suspension of 5.73 g (50 mmoles) of 1-methyl-2-mercapto-imidazole in absolute ethanol (100 ml) is added with 2,6-lutidine in catalytic amount and there is dropwise added the solution of isobutyl p-(2,3-epoxy)-propyloxybenzoate (12.5 g; 50 mmoles) in absolute ethanol (50 mmoles) at room temperature under stirring. The mixture is heated to reflux for 6 hours. The solvent is evaporated under vacuum, the residue is taken with ethyl acetate and washed with aqueous saturated solution of sodium bicarbonate and with water. The mixture is made anhydrous over anhydrous sodium sulfate and concentrated to an oil. The lutidine is completely removed by evaporation under vacuum. The product, dissolved in acetone, is treated with an excess of 37% aqueous hydrochloric acid and maintained under stirring until the salification is completed. The mixture is concentrated to dryness under vacuum with subsequent additions of toluene/ethanol, the solid is comminuted with ethyl ether/hexane and is crystallized from a mixture of acetone/ethyl acetate. The product is obtained with a yield of 64% and has melting point 104-108 C. By repeating the operating method of example 4 the following derivatives are prepared:

The synthetic route of 1-Methyl-1H-imidazole-2(3H)-thione has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pierrel SpA; US5470858; (1995); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Adding a certain compound to certain chemical reactions, such as: 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, belongs to imidazoles-derivatives 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 60-56-0, SDS of cas: 60-56-0

General procedure: To a slurry of the substituted imidazole-2-thione or pyrimidine-2-thiol (1.0 mmol) and sodium methoxide (2.2 mmol) in methanol (20 mL) was added a solution of substituted 2-(chloromethyl)-pyridine (1.0 mmol) in methanol (10 mL). After the mixture was refluxed with stirring for 4-6 h, the solvent was removed in vacuo and the residue was washed with water to remove the salt, and then extracted with dichloromethane (3 9 10 mL) at room temperature. The solid product was directly obtained by the removal of solvent and further dried at 45 C overnight. The purity of the product was tested by HPLC and characterization of the product was confirmed by IR, 1H NMR, and mass spectroscopies. Data 3-Methyl-[4-(2,2,2-Trifluoroethoxy)-2-Pyridinyl]-Methylthio-1-Methyl-Imidazole (3a) White solid. Yield: 84.5 %. IR (cm-1): 832.7 (-CH2-S-). 1H NMR (CDCl3) delta (ppm): 2.18 (s, 3H, -CH3 in py), 3.23 (s, 3H, -CH3 in imidazole), 4.42 (q, J = 6.0 Hz, 2H,-OCH2CF3), 4.56 (s, 2H, -CH2S-), 6.62 (d, J = 5.6 Hz,1H, H in py), 6.81 (s, 1H, H in imidazole), 6.92 (s, 1H,H in imidazole), 8.30 (d, J = 5.6 Hz, 1H, H in py). MS (EI): m/z calcd. C13H14N3OF3S (M+) 317.3311, found 317.3336.

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; Ma, Sen; Jia, Ai-Quan; Fan, Fang-Fang; Shi, Hua-Tian; Zhang, Qian-Feng; Journal of Chemical Crystallography; vol. 46; 3; (2016); p. 137 – 143;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

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. 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, This compound has unique chemical properties. The synthetic route is as follows., Safety of 1-Methyl-1H-imidazole-2(3H)-thione

General procedure: To a stirred suspension of potassium carbonate (0.166 g, 1.2mmol) in ethanol (8 mL) was added 1H-imidazole (0.068 g,1 mmol). The mixture was stirred at 60 C for 1 h and thencooled to room temperature. Compound 3 (0.232 g, 1 mmol)was added and stirred under 70 C. After the reaction wascompleted (monitored by TLC, chloroform/methanol, 30:1,V/V), the solvent was evaporated and the residue was treatedwith water (15 mL) and extracted with chloroform (315mL). The combined organic phase was dried over anhydroussodium sulfate and concentrated under the reduced pressure.The crude product was purified by silica gel column chromatography(eluent, chloroform/methanol, 50:1-30:1, V/V)to afford the pure compound 4a (0.142 g) as white solid

According to the analysis of related databases, 60-56-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Peng, Xin-Mei; Kumar, Kannekanti Vijaya; Damu, Guri L.V.; Zhou, Cheng-He; Science China Chemistry; vol. 59; 7; (2016); p. 878 – 894;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

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 60-56-0 as follows. Quality Control of 1-Methyl-1H-imidazole-2(3H)-thione

Dithiafulvalenyl compound 1 (0.2 mmol), mercapto-thiazole 2 (2 mmol, 10 equiv.), and I2 (0.6 mmol, 3 equiv., 152.4 mg) were dissolved in DMSO (3 mL). The reaction mixture was stirred at 25 C for 12 h under N2 atomsphere. Then quenched with a saturated solution of Na2S2O3 and stirred for half an hour, the solution was extracted with dichloromethane (CH2Cl2). The organic layer was separated, and dried over Na2SO4. Then the organic solvent was removed in vacuo to afford the respective thiadiazole-based dithiafulvalene (DTF) derivatives (3), which were purified by column chromatography (silica gel, PE / CH2Cl2) to afford pure substances.

According to the analysis of related databases, 60-56-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Fu, Huimin; Zhao, Bangtun; Zhu, Weimin; Tetrahedron Letters; vol. 60; 2; (2019); p. 124 – 128;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

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. 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1-Methyl-1H-imidazole-2(3H)-thione

General procedure: A mixture of tosylhydrazone 1 (1 mmol), thiol 2 (1.5 mmol, 1.5 equiv), K2CO3 (2.5 mmol, 2.5 equiv) in toluene (4.0 mL) was stirred at 100 C for 24h under Argon. After completion of the reaction as indicated by TLC, the mixture was cooled to room temperature. After adding CH2Cl2 (10 mL), the organic phase was washed with saturated NaHCO3, brine and dried with Na2SO4, and concentrated under reduced vacuum. The residue was then purified by flash chromatography on silica gel to afford product 3.

According to the analysis of related databases, 60-56-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Garcia-Carrillo, Mario Alfredo; Guzman, Angel; Diaz, Eduardo; Tetrahedron Letters; vol. 58; 20; (2017); p. 1952 – 1956;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Electric Literature of 60-56-0,Some common heterocyclic compound, 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, molecular formula is C4H6N2S, 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 7-[4-(2-butoxyethoxy)phenyl]-N-[4-(hydroxymethyl)phenyl]-1-isobutyl-2,3-dihydro-1-benzazepine-4-carboxamide (500 mg) in THF (10 ml) was added 1 droplet of pyridine, and thionyl chloride (0.09 ml) was added to the mixture at 0C. The mixture was allowed to be at room temperature under nitrogen atmosphere, and stirred for 1 hour. The solvent and excess thionyl chloride were distilled off under reduced pressure, and the residue was dissolved in THF (10 ml). This solution was added to a solution of 2-mercapto-1-methylimidazole (137 mg) and triethylamine (1.67 ml) in THF (10 ml) at 0C, and the mixture was heated overnight under nitrogen atmosphere at 50C. The mixture was allowed to be cooled, water was added to the mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure. The obtained residue was separated and purified by silica gel column chromatography (hexane:ethyl acetate = 1:2), to give 7-[4-(2-butoxyethoxy)phenyl]-1-isobutyl-N-[4-[[(1-methylimidazol-2-yl)sulfanyl]methyl]phenyl]-2,3-dihydro-1-benzazepine-4-carboxamide (437 mg) (Compound 358) as yellow amorphous. 1H-NMR (200 MHz, CDCl3) delta 0.90 to 0.99 (9H, m), 1.30 to 1.45 (2H, m), 1.50 to 1.70 (2H, m), 1.95 to 2.20 (1H, m), 2.90 to 2.97 (2H, m), 3.19 (2H, d, J = 7.4 Hz), 3.28 (3H, s), 3.30 to 3.40 (2H, m), 3.55 (2H, t, J = 6.6 Hz), 3.80 (2H, t, J = 4.6 Hz), 4.13 to 4.18 (4H, m), 6.87 to 7.11 (7H, m), 7.37 to 7.56 (8H, m). Elemental Analysis for C38H46N4O3S·0.3H2O Calcd. C, 70.84; H, 7.29; N, 8.70; Found. C, 70.62; H, 7.49; N, 8.91.

The synthetic route of 60-56-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Chemical Industries, Ltd.; EP1422228; (2004); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Electric Literature of 60-56-0, 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. 60-56-0 name is 1-Methyl-1H-imidazole-2(3H)-thione, 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.

General procedure: A mixture of 3-chloromethyl-4-methoxybenzaldehyde (2a) (1.85 g, 0.01 mol), the corresponding phenol or thiol (0.011 mol), and potassium carbonate (2.00 g, 0.0145 mol) in a mixture of acetonitrile-DMF (20 mL, from 9 : 1 to 8 : 2, v/v) was refluxed for 5-7 h withstirring (TLC monitoring). After evaporation of the solvents, the residue was treated with water, a precipitate formed was filtered off, washed with 40% aqueous ethanol, and dried in air. Yields and physicochemical characteristics of aldehydes 5a-m and 6a-g are given in Table 2.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-1H-imidazole-2(3H)-thione, and friends who are interested can also refer to it.

Reference:
Article; Khachatryan; Razinov; Kolotaev; Belus?; Matevosyan; Russian Chemical Bulletin; vol. 64; 2; (2015); p. 395 – 404; Izv. Akad. Nauk, Ser. Khim.; 2; (2015); p. 395 – 404,10;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, belongs to imidazoles-derivatives 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: 60-56-0

Triethylamine (0.0749 g, 0.75 mmol) was added to a solution of2-mercapto-1-methylimidazole (0.0856 g, 0.75 mmol) in tetrahydrofuran(15 mL) and the mixture was stirred for 30 min at roomtemperature. Then, 1-(bromomethyl)pyrene (0.1476 g, 0.5 mmol)was slowly added and the reaction mixture was heated underreflux for 24 h. After cooling to room temperature, the mixture wasfiltered and the solvent was evaporated, the crude residue waspurified by column chromatography (1:1 ethyl acetate/petroleumether) to obtain a brown solid of compound 2 (0.1301 g, 79.3%yield). Characterization of compound 2: 1H NMR600 MHzd6-DMSO3.62 (s, 3H), 3.87 (d, 2H), 7.12 (s, 1H), 7.45 (s, 1H), 7.63(dd, 2H), 8.15 (m, 1H), 8.28 (d, 1H), 8.32 (m, 2H), 8.36 (m, 2H), 8.38(d, 1H), 8.50 (d, lH). Mass spectra (Fig. S2): calculated for C21H16N2S[M+H]+, 329.1; found, 328.81.

The synthetic route of 60-56-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Jing; Jiang, Huihui; Liu, Hai-Bo; Liang, Lebao; Tao, Junrong; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 228; (2020);,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem