Month: May 2021

Application of 15813-07-7, The chemical industry reduces the impact on the environment during synthesis 15813-07-7, name is 5-Iodo-4-methyl-1H-imidazole, I believe this compound will play a more active role in future production and life.

To a stirred solution of 4-lodo-5-methyl-1 H-imidazole (5g, 24mmol) in THF (100mL) cooled to 0C was added sodium hydride (60% dispersed in mineral oil) (1 .06g, 26mmol), the resulting suspension was stirred for 1 hr at this temperature. 2-(Trimethylsilyl)ethoxymethyl chloride (4.25ml_, 24mmol) was added slowly and the solution was allowed to warm to room temperature overnight. Further Sodium hydride (60% dispersed in mineral oil) (0.5 eq) was added and the solution was stirred for 1 .5hr. A small amount of water was added before the the solution was concentrated in vacuo. Water and DCM were added and the solution partitioned. The aqueous layer was washed with further DCM (x2) before the combined organics were passsed through a phase separator and concentrated to dryness in vacuo to afford a dark yellow oil. The residue was dissolved in DCM and purified by flash column chromatography (80g S1O2, 0-50% EtOAc in Heptane). TLC still showed both regioisomers together in all fractions so the fractions were concentrated to dryness in vacuo to afford 2-[(4-iodo-5-methyl-imidazol-1 -yl)methoxy]ethyl-trimethyl-silane and 2-[(5-iodo-4-methyl- imidazol-1 -yl)methoxy]ethyl-trimethyl-silane in a ratio of 1 : 0.6 in favour of the title product (5.59g, 17mmol, 69% yield) as a yellow oil. MS Method 2: RT: 1 .44 min, ES+ m/z 339.1 [M+H]+ and 1 .84 min, ES+ m/z 339.1 [M+H]+ H NMR (400MHz, CDCb) delta/ppm: 7.73 ( s, 1 H, minor), 7.49 (s, 1 H, major), 5.22 (s, 2H, both regioisomers), 3.40-3.50 (m, 2H, both regioisomers), 2.27 (s, 3H, major), 2.26 (s, 3H, minor), 0.85- 0.93 (m, 2H, both regioisomers), 0.03 (s, 9H, both regioisomers).

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, 5-Iodo-4-methyl-1H-imidazole, other downstream synthetic routes, hurry up and to see.

Electric Literature of 1450-93-7, A common heterocyclic compound, 1450-93-7, name is 1H-imidazol-2-amine sulfate(2:1), molecular formula is C6H12N6O4S, 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.

C. A mixture of 2-((5S)-5-(3-(cyclopentyloxy)-4-methoxyphenyl)-2- oxopiperidin-3-yl)acetic acid (218 mg, 0.63 mmol), 2-aminoimidazole sulfate (83 mg, 0.63 mmol), BOP (278 mg, 0.63 mmol) and N,N-diisopropylethylamine (0.33 mL, 1.89 mmol) in dry DMF (5 mL) was stirred at 60 0C under argon for six hours. The mixture was diluted with water and the resulting solution was extracted with EtOAc (4x). The combined organic layer was washed with brine, dried over MgSO4, filtered and the filtrate was evaporated to dryness. The residue was purified by radial chromatography (0% to 5% methanol in CH2CI2) to give 2-[(5S)- 5-(3-cyclopentyloxy-4-methoxyphenyl)-2-oxo-3-piperidinyl]-N-(2-imid- azolyl)acetamide as a mixture of diastereomers (119 mg, 46%) as a white solid.

The synthetic route of 1450-93-7 has been constantly updated, and we look forward to future research findings.

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. 53484-16-5, name is 6-Bromo-1-methyl-1H-benzo[d]imidazole, A new synthetic method of this compound is introduced below., Formula: C8H7BrN2

A microwave flask was charged with copper(l) chloride (1.87 g, 18.95 mmol), copper(l) iodide (0.36 g, 1.895 mmol) and 6-bromo-1-rnethyl-benzirnidazole (2.00 g, 9.48 mmol), and the vial was flushed with nitrogen. NMP (18 mL) was added. The flask was heated under microwave irradiation to 200 0C for 1.5 h. The mixture was diluted with ethyl acetate (1.5 L) and a 9:1 saturated aqueous ammonium chloride- ammonium hydroxide solution was added (0.25 L). The mixture was stirred vigorously for 15 min and filtered through celite. The two phases were separated and the organic phase was washed with water (0.2 L*5). The combined organic phase was dried over MgSO4, filtered and concentrated to give a moist pale brown solid, contaminated with NMP. The solid was redissolved in ethyl acetate and washed with water. The organic phase was dried over MgSO4, filtered and concentrated to give 6-chloro-1-methyl-1H-benzo[d]imidazole. ESI- MS: m/z 167.1, (M+H)*.

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 of 288-32-4,Some common heterocyclic compound, 288-32-4, name is 1H-Imidazole, molecular formula is C3H4N2, 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 ofnitrogen-containing nucleophile (1 eq.) and cesium carbonate (3.0 eq.) in N,N-dimethylformamide (2 mL/mmol) was added 2-haloheterocycle (1.1 eq.). Thereaction was heated to 100 C. and stirred at this temperature for 2 hours. Thereaction was then cooled to room temperature and acidified to pH=1 with 10%aqueous HCl solution if product contains a carboxylic acid, or diluted withwater if neutral. The solution was extracted with twice with dichloromethane.The organic layers were combined, dried with sodium sulfate and concentratedunder vacuum. The crude material was either used directly in subsequentreactions or purified by flash chromatography.

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

Reference of 16042-25-4, These common heterocyclic compound, 16042-25-4, name is 2-Imidazolecarboxylic 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.

PREPARATION 35 1-amino-N-o-tolyl-1H-imidazole-2-carboxamide a) N-o-tolyl-1H-imidazole-2-carboxamide To a solution of 1H-imidazole-2-carboxylic acid (0.52 g, 4.64 mmol) in DMF (20 mL) was added o-toluidine (0.50 mL, 4.64 mmol), EDC·HCl (1.35 g, 6.96 mmol) and HOBt (0.94 g, 6.96 mmol). The reaction mixture was stirred at room temperature for 16 hours. Then, it was poured into water and extracted with ethyl acetate. The combined organic layer was dried over sodium sulphate, filtered and concentrated to dryness. The crude product was purified by flash chromatography (2% to 3% MeOH/DCM) to yield 0.93 g (99%) of the title compound as a beige solid. LRMS (m/z): 202 (M+1)+.

Statistics shows that 2-Imidazolecarboxylic acid is playing an increasingly important role. we look forward to future research findings about 16042-25-4.

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. 540516-28-7, name is 2-(Hydroxymethyl)-5-bromobenzimidazole, A new synthetic method of this compound is introduced below., Safety of 2-(Hydroxymethyl)-5-bromobenzimidazole

Example 15. Production of intermediate compounds (l-amino-5-bromo-lH- benzimidazol-2-yl)methanol (compound 17) and (l-amino-6-bromo-lH-benzimidazol-2- yl)methanol (compound 18).The 5(6)-bromo-lH-benzimidazol-2-methanol (16 a, b) (5.2 g, 22.7 mmol), prepared to known methodology, is dissolved in a solution of KOeta (4.8 g, 72.8 mmol) in H2O (40 niL). To the mixture is added under stirring at 400C solution Of NH2OSO3H (6g, 50mmol) in H2O (15 mL), neutralized NaHCO3. Upon the completion of the exothermal reaction the mixture is still incubated at 40-500C for 0.5 h and then cooled to room temperature. The resultant precipitate is filtered and recrystallization is accomplished from water. The mixture of compounds 17 and 18 is obtained in 1 :1 ratio (according to 1H NMR). The mixture of these compounds is crystalline, white.Overall yield: 3.7g (67%). 1H NMR (300 MHz, DMSO-d6): delta ppm 4.73 (4H, s, 2CH2), 5.43 (IH, s, OH), 5.45 (IH, s,OH), 6.01 (2H, s, NH2), 6.03 (2H, s, NH2), 7.31 (IH, d, J- 9Hz, ArH), 7.39 (IH, d, J= 9Hz, ArH), 7.46 (IH, d, J- 9Hz, ArH), 7.53 (IH, d, J= 9Hz, ArH), 7.67 (IH, s, ArH), 7.73 (IH, s, ArH).13C NMR (75 MHz, DMSO-d6): delta ppm 55.81, 55.81, 112.48, 113.46, 114.15, 114.98, 121.46, 122.01, 124.93, 125.36, 135.73, 137.78, 139.62, 141.88, 156.17, 156.48. IR (v, cm”1): 3350, 3313, 3184, 3120 NH2.Analysis (C8H8BrN3O): calcd: C 39.67%, H 3.31 %, N 17.36%; found: C 39.88%, H 3.52%, N 17.46%.

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.

Synthetic Route of 106429-57-6, 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. 106429-57-6, name is Methyl 2-oxo-2,3-dihydro-1H-benzo[d]imidazole-5-carboxylate belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

methyl 2-oxo-2,3-dihydro-1H-1,3-benzimidazole-5-carboxylate (1.3 g, 6.6 mmol), pyridine hydrobromide (1.0 g, 6.6 mmol) and phosphorous oxybromide (3.7 g, 13 mmol) were mixed in EtOAc (100 ml). The reaction mixture was stirred at reflux for 7 d. Water was added. The organic phase was washed with NaHC03 (sat., aq), dried over MgS04, filtered and concentrated. The intermediate methyl 2-bromo-1H-benzimidazole-6-carboxylate was obtained in 100% yield (1.6 g). MS (ESI+) m/z 255 [M+H]+. HPLC purity: 95%. 1H NMR (600 MHz, MeOD- ) delta ppm 8.21 (s, 1 H) 7.96 (dd, J=8.55, 1.53 Hz, 1 H) 7.58 (d, J=8.55 Hz, 1 H) 3.93 (s, 3 H)

The synthetic route of Methyl 2-oxo-2,3-dihydro-1H-benzo[d]imidazole-5-carboxylate has been constantly updated, and we look forward to future research findings.

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. 96797-15-8, name is 4-Iodo-1-trityl-1H-imidazole belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C22H17IN2

Step 11C 62ATo a solution of 4-iodo-trityl-imidazole (6.77 g, 15.5 mmol) in DCM (100 ml_) was added EtMgBr (3.0M in Et2O, 4.96 mL, 14.9 mmol) slowly at -200C, stirred at – 200C for 30 min. A solution of 1C (2.8 g, 13.5 mol) in DCM (20 mL) was added very slowly. The mixture was stirred at RT for 1 h, quenched with saturated NH4CI, diluted with DCM. The DCM layer was washed with brine, dried and concentrated. Flash chromatography (EtOAc/Hexanes, 1 :2 then 10:1 ) afforded 62A (5.0 g, 72%).

The synthetic route of 96797-15-8 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 75370-65-9, These common heterocyclic compound, 75370-65-9, name is 4-Amino-1H-benzo[d]imidazol-2(3H)-one, 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.

Commercially available p-chlorobenzylamine (846 mg, 6 mmol) was dissolved in 40 ml of AcOEt and at 0C triphosgene (1.78 g, lequiv.) was added to the solution. The mixture was warmed at 80C for 4 hours then evaporated and the residue was dissolved in 20 ml of DMF. The solution of the isocyanate was added dropwise to a solution in DMF (10 ml) of compound la (900 mg, 6 mmol) and the mixture was warmed at 80C for 8 hours. (TLC AcOEt). The solvent was evaporated and the crude was dissolved in AcOEt (50 ml) and washed with water (1 X 30 ml) and brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The purification of the crude residue by chromatographic column gave 300 mg of a white solid. Yield = 16% ‘HNMR (DMSO, 200 MHz) delta 4.30 (2H, d, J = 6.2 Hz), 6.62 (1H, dd, J = 7.6 Hz, J’ = 1.2 Hz), 6.83 (2H, m), 6.96 (1H, dd, J = 8 Hz, J’ = 1 Hz), 7.35 (4H, m), 8.27 (1H, bs), 9.98 (1H, bs), 10.59 (1H, bs); [M+1] 317.1 (C15H13ClN4O2 requires 316.74).

The synthetic route of 75370-65-9 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 10111-08-7, These common heterocyclic compound, 10111-08-7, name is Imidazole-2-carboxaldehyde, 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.

In DMF (15 ml), 2-imidazole carboxaldehyde (500 mg) was dissolved. Then, the solution was added with iodoethane (1.25 ml) and sodium hydride (208 mg), followed by stirring at room temperature for 5 days. After completion of the reaction, the solvent was distilled off and the residue was then added with chloroform, followed by washing with water and saturated saline solution. The resultant was dried with anhydrous sodium sulfate, and the solvent was then distilled off. The residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (280 mg) as a yellow oily substance. 1H-NMR(500MHz,DMSO-d6):delta=1.44(3H,t,J=7.3Hz),4.44 (2H,q,J=7.3Hz),7.18(1H,s),7.29(1 H,s),9.82(1H,s).

The synthetic route of 10111-08-7 has been constantly updated, and we look forward to future research findings.