Month: April 2021

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. 1003-21-0, name is 5-Bromo-1-methyl-1H-imidazole, A new synthetic method of this compound is introduced below., Product Details of 1003-21-0

To a solution of 5-bromo-1-methyl-1H-imidazole (0.074 g, 0.46 mmol) in DCM (5 mL) was added ethyl magnesium bromide (0.153 mL, 0.46 mmol; 3M in diethyl ether) dropwise over a 10 minute period. The resulting cloudy mixture was stirred at room temperature for 20 minutes, cooled in an ice bath to 0 C. and (4-chloro-2-methoxy-3-(4-(methylsulfonyl)benzyl)quinolin-6-yl)(4-chlorophenyl)methanone (0.10 g, 0.20 mmol, Intermediate 22: step b) dissolved in THF (3 mL) was added. The cold bath was removed and the reaction mixture stirred at room temperature for 10 minutes then heated in an 80 C. oil bath for 16 hours. The mixture was cooled to room temperature, H2O added followed by 6M aqueous HCl to a neutral pH. The aqueous mixture was extracted with DCM (2*). The combined DCM extracts were dried over Na2SO4, filtered, concentrated under reduced pressure, chromatographed (0-10% MeOH in CH2Cl2) then further purified by Gilson HPLC(H2O/acetonitrile/1% TFA) to afford the title compound as a white solid. 1H NMR (400 MHz, DMSO-d6) delta ppm 3.17 (s, 3H) 3.53 (s, 3H) 4.03 (s, 3H) 4.36 (br. s., 2H) 6.96 (s, 1H) 7.38 (d, J=8.59 Hz, 2H) 7.48 (t, J=8.84 Hz, 4H) 7.55-7.68 (m, 2H) 7.76-7.94 (m, 3H) 8.11 (s, 1H) 9.12 (br. s., 1H); MS (ESI) 582.

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.

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. 288-32-4, name is 1H-Imidazole, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C3H4N2

General procedure: To a solution of 1 (0.02 mmol) in H2O/MeCN (v/v=2/1, 4 mL) was added 1H-imidazole (1.0 mmol) and arylboronic acid (2 mmol)under O2 atmosphere. The mixture was stirred at 60 C for 24 h. After cooling to ambient temperature, the mixture was partitioned between water and CH2Cl2. The organic layer was separated, and the aqueous layer was extracted with CH2Cl2. The combined organic layers were washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash chromatography on silica gel.

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 288-32-4.

Electric Literature of 41716-18-1,Some common heterocyclic compound, 41716-18-1, name is 1-Methyl-1H-imidazole-4-carboxylic acid, molecular formula is C5H6N2O2, 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 solution of 1-methyl-1Himidazole-4-carboxylic acid (0.50 g, 4.0 mmol), 1-hydroxybenztriazole monohydrate (0.74 g, 4.8 mmol), and 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (0.92 g, 4.8 mmol) in acetonitrile (10 mL) was added a solution of 3-(trifluoromethoxy) benzylamine 8(0.84 g, 4.4 mmol) in acetonitrile (10 mL), and the mixture was stirred at room temperature for overnight. The reaction mixture was concentrated in vacuo, and saturated aqueous NaHCO3solution was added to the residue. After extraction with ethyl acetate, the organic layer was dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The residue was purified using silica gel column chromatography (0?10percent MeOH in CHCl3) to obtain 9(1.18 g, 98percent) as a colorless powder

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-4-carboxylic acid, its application will become more common.

Synthetic Route of 24134-09-6, 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 24134-09-6 as follows.

Preparation 163 4-(1,2-dimethyl-1H-imidazol-5-yl)aniline Tetrakis(triphenylphosphine)palladium (0.053 g, 0.046 mmol) was added to a solution of 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (0.1 g, 0.456 mmol), 5-bromo-1,2-dimethyl-1H-imidazole (0.088 g, 0.502 mmol) and cesium fluoride (0.208 g, 1.369 mmol) in DME/MeOH (2/1, 2.9 mL). The reaction mixture was heated for 10 minutes at 150 C. under microwave irradiation. The reaction was diluted with EtOAc and quenched with water. The layers were separated and the aqueous layer was extracted with EtOAc. The combined organic layers were dried (Na2SO4), filtered and concentrated under reduced pressure. The crude mixture was purified using Biotage silica gel column chromatography eluting with 1 to 5% MeOH/aq. NH3 (10/1) in DCM followed by filtration through a SCX-2 column to afford the title product as a white solid (48 mg, 56%). 1H NMR (500 MHz, CDCl3): delta 2.42 (s, 3H), 3.46 (s, 3H), 3.81 (br s, 2H), 6.71-6.74 (m, 1H), 6.85 (s, 1H), 7.12-7.14 (m, 1H). LC (Method B)-MS (ESI, m/z) tR 0.24 min, 188 [M+H]+

According to the analysis of related databases, 24134-09-6, the application of this compound in the production field has become more and more popular.

Application of 5805-57-2, The chemical industry reduces the impact on the environment during synthesis 5805-57-2, name is (1H-Benzo[d]imidazol-2-yl)methanamine, I believe this compound will play a more active role in future production and life.

The residue was dissolved in DMF and EDC (0.15 rnmol), HOBt (0.1 rnmol), DIPEA (0.25 rnmol), ( lH-benzo[d]imidazol-2- yl)methanamine (0.1 rnmol) were added. The solution was stirred at room temperature overnight and then removed under vacuum. ‘T’he residue was dissolved in EtOAc (25 mL). The organic layer was washed with water, brine (25 mL), dried and concentrated under vacuum. The residue was chromatographed to give N-((lH-benzo[d]iniidazoi-2-yl)ineihyi)-2- (5,7-dichloro- 1 H-benzo[d]imidazol-2-yl)acetamide (1764). LC/MS: (EST) (M +H)+= 375.6.

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, (1H-Benzo[d]imidazol-2-yl)methanamine, other downstream synthetic routes, hurry up and to see.

Reference of 33016-47-6, The chemical industry reduces the impact on the environment during synthesis 33016-47-6, name is 1-Trityl-1H-imidazole-4-carbaldehyde, I believe this compound will play a more active role in future production and life.

1-Trityl-1H-imidazole-4-carboxaldehyde (Daminos-Zeghal S. et al., Tetrahedron, 1997, 53(22), 7605-14) (5 g; 14.8 mmol) is dissolved in dichloromethane (35 ml) under a nitrogen atmosphere and then cooled to -78 C. Methyl trifluoromethanesulfonate (1.7 ml; 14.8 mmol) is added dropwise and the reaction mixture is allowed to warm slowly to room temperature (over 2 hours). Phosphate buffer solution (pH 7; 50 ml) is added and the two-phase mixture is stirred vigorously for 15 minutes. The two phases are then separated and the aqueous phase is extracted three times with dichloromethane. The organic phases are combined, dried over magnesium sulfate, filtered and concentrated. The orange-colored solid obtained is purified by flash chromatography (CH2Cl2, then 10/90 acetone/CH2Cl2 and then 5/95 MeOH/CH2Cl2) to give the desired product (1.39 g; 85%). [0250] 1H NMR, DMSO-d6 (ppm): 3.87 (s, 3H); 7.88 (s, 1H); 8.00 (s, 1H); 9.75 (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, 1-Trityl-1H-imidazole-4-carbaldehyde, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 78162-58-0, name is N,N-Dimethyl-1H-imidazole-1-sulfonamide, 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 78162-58-0, Product Details of 78162-58-0

EXAMPLE H Procedure for Preparation of 4(5)-phenylsulfanyl-1H-imidazole: Procedure 1-(N,N-dimethylsulfamoyl)imidazole (1.5g, 8.6 mmol) was taken up in 28mL of THF. The solution was cooled to -78 C. and n-BuLi (5.4mL, 8.6 mmol) added dropwise via syringe. After stirring at -78 C. for 1h TBSCl (1.3g, 8.56 mmol) in 10mL of THF was added. The bath was removed and the reaction allowed to warm-up to rt. The reaction mixture was stirred overnight. The reaction mixture was cooled to -20 C. and n-BuLi (5.4 mL, 8.6 mmol) added. After 45 min phenyldisulfide (1.9g, 8.6 mmol) in 8mL of THF was added. The reaction mixture was stirred at rt for 48h. The reaction mixture was quenched with saturated ammonium chloride and extracted with ethyl acetate. The organic layer was collected and washed with water and then brine. The solution was dried over sodium sulfate and the solvent removed under reduced pressure. Flash chromatography (2.5% EtOAc/hexane) afforded 2.8g (7.0 mmol) of 2-(t-butyldimethylsilyl)-5-phenylsulfanylimidazole-1-sulfonic acid dimethylamide (1) as a yellow color oil.

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, N,N-Dimethyl-1H-imidazole-1-sulfonamide, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 40197-20-4, name is 5-Bromo-1H-benzo[d]imidazole-2-carboxylic 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. COA of Formula: C8H5BrN2O2

N-[3-(dimethylamino)propyl]-N?-ethylcarbodiimide hydrochloride (1.2 g) was added to a mixture of 5-bromo-1H-benzimidazol-2-carboxylic acid (1.0 g), 1-[4-(trifluoromethyl)benzyl]piperazine (1.0 g), 1H-benzotriazol-1-ol (840 mg), and N,N-dimethylformamide (10 ml: hereinafter, abbreviated as DMF), followed by stirring at room temperature overnight. A saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture, followed by stirring at room temperature for 1 hour, and the resulting solid was collected by filtration, followed by drying under reduced pressure. The obtained solid was dissolved in a mixture of chloroform (100 ml) and ethanol (1 ml) while heating to reflux. The mixture was cooled to room temperature and then hexane (100 ml) was added thereto. The resulting solid was collected by filtration, followed by drying under reduced pressure, thereby obtaining (5-bromo-1H-benzimidazol-2-yl){4-[4-(trifluoromethyl)benzyl]piperazin-1-yl}methanone (1.4 g) as a solid.

The synthetic route of 5-Bromo-1H-benzo[d]imidazole-2-carboxylic acid has been constantly updated, and we look forward to future research findings.

Electric Literature of 152628-02-9,Some common heterocyclic compound, 152628-02-9, name is 1,7′-Dimethyl-2′-propyl-1H,1’H-2,5′-bibenzo[d]imidazole, molecular formula is C19H20N4, 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.

Compound c, represented by Formula 3, was synthesized using Compound a and Compound b purified in Example 1-1. Lithium tert-butoxide was reacted in an inexpensive t-BuOH (tert-butyl alcohol) solvent to obtain compound c in a yield of 54%. As a result of comparing various base conditions such as pyridine, DMAP, Et3N, K2CO3, KOAc, NaOEt, NaH, and Na / MeOH, Compound c was obtained in a yield of 66% at a room temperature of Na / MeOH and 71% at 70 C. Also, a reaction of 1 g scale was carried out to synthesize compound c in the final 70% yield. Then, in order to hydrolyze the obtained compound c, hydrolysis optimum reaction conditions were searched under various acid or base conditions.The reaction was detected in the acid hydrolysis conditions of HCl / CH2Cl2 or H2SO4 / H2O, but the yield was not improved, and the hydrolysis reaction was carried out using the base conditions.The reaction was optimized using sodium hydroxide (NaOH) and THF, DMSO, toluene or H2O solvent, and 3N NaOH / THF at 100 was selected. As a result, telmisartan, a compound represented by the following formula (4), was obtained in a yield of 93%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,7′-Dimethyl-2′-propyl-1H,1’H-2,5′-bibenzo[d]imidazole, its application will become more common.

Electric Literature of 615-16-7,Some common heterocyclic compound, 615-16-7, name is 2-Hydroxybenzimidazole, molecular formula is C7H6N2O, 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 three flask equipped with a thermometer dichloroethane solvent 1000ml, added slowly with stirring 268gBenzimidazolone. Meanwhile weighed 305g of fuming nitric acid (concentration ?95%), and slowly poured three bottles, while down while stirring. Then added phosphorus pentoxide 20g. Reflux, the reaction temperature is 85 , TLC tracking dinitro compound detected is generated to stop the reaction. While recovering the solvent was concentrated under reduced pressure, water was added, extraction dichloroethane, and the solvent was evaporated to dryness to give the product recovered organic phase was dried over anhydrous sodium sulfate. 381g dried to give a solid, a yield of 85.1%.

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