Month: April 2021

Electric Literature of 6851-80-5, These common heterocyclic compound, 6851-80-5, name is 1-(2-Methoxyphenyl)-N-methylmethanamine, 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: To a mixture of the corresponding secondary amines 14A-F (0.6 mmol), anhydrous K2CO3 (89.7 mg, 0.65 mmol) and KI (8.6 mg, 0.052 mmol) in anhydrous CH3CN (12 ml) were added the appropriate intermediates 10-13 (0.5 mmol). The reaction mixture was warmed to 60-65 C and stirred for 6-10 h under an argon atmosphere. After complete reaction, the solvent was evaporated under reduced pressure. The residue was dissolved in water (40 mL) and the mixture was extracted with dichloromethane (25 mL×3). The combined organic phases were washed with saturated aqueous sodium chloride (20 mL), dried over sodium sulfate, and filtered. The solvent was evaporated to dryness under reduced pressure. The residue was purified on a silica gel chromatography using mixtures of CH2Cl2/CH3OH (100:1) as eluent to afford the corresponding scutellarein-O-alkylamine derivatives 15-18.

The synthetic route of 6851-80-5 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 20469-65-2, name is 1-Bromo-3,5-dimethoxybenzene, 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. SDS of cas: 20469-65-2

A 200-mL two-neck round-bottom flask was charged with anitrogen atmosphere, and to the flask, 1-bromo-3,5-dimethoxybenzene (2.92 g, 13.82 mmol), bis(pinacolato)diboron (5.26 g, 20.73 mmol), Pd(dppf)Cl2?CH2Cl2 (1.56 g, 1.91 mmol) and KOAc (2.10 g, 20.73 mmol) were added into 80 mL of dry DMF. The mixture was stirred at 80C for 60 h under nitrogen. Then, DMF was removed by vacuum distillation, and the residue was extracted with CH2Cl2 (3 20 mL). The CH2Cl2 layer was washed with H2O (2 x 20 mL), dried over anhydrous Na2SO4, filtered and concentrated in vacuo to give a brown crude. The crude product was purified by column chromatography on silica gel (eluent: EtOAc: hexane, 2/3 v/v) to give white compound as a first band. (1.16 g, 88%). 1H-NMR (500 MHz, DMSO) delta(ppm)= 6.95(2H, d, J= 2.6 Hz), 6.57 (1H, t, J= 2.5 Hz), 3.81 (6H, s), and 1.34 (12H, s).

The synthetic route of 1-Bromo-3,5-dimethoxybenzene has been constantly updated, and we look forward to future research findings.

Reference of 578-57-4, 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. 578-57-4, name is 1-Bromo-2-methoxybenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: CuI (0.05 mmol), aryl halide (0.5 mmol), Na3PO4 (0.5 mmol), 25-28% aqueous ammonia (1 mL), and PEG-400 (2 mL) were added to a sealed tube. The reaction mixture was stirred at 100 C (aryl iodides for 15 h and aryl bromides for 24 h) and then cooled to room temperature and extracted with diethyl ether (3 times). The combined organic phase was then dried with anhydrous Na2SO4 and the solvent was removed under reduced pressure. The remaining residue was purified by column chromatography on silica gel to provide the desired aryl amines.

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

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. 22483-09-6, name is 2,2-Dimethoxyethanamine, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2,2-Dimethoxyethanamine

A solution of 2-thiophenecarboxaldehyde (Ig, 8.93mmol) and aminoacetaldehyde dimethylacetal (1.4g, 13.4mmol) in DCM (23OmL) was stirred at 350C for 1 h.Sodium triacetoxyborohydride (5.68g, 27mmol) was added and the reaction stirred at r.t. for 5 hours. NaHCO3 (saturated solution, 10OmL) was added and the organics were collected, washed (brine), dried (MgSO4) and concentrated in vacuo. The residue was purified via flash chromatography eluting with 50% EtOAc/isohexane to afford the title compound as a yellow oil. Yield 1.6g (90%): HPLC retention time, 2.76min (Solvent: CH3CN/H2O/0.05% NH3, 5-95% gradient H2O-6min. Column: EPO Xterra 50 x 4.60 i.d., Cl 8 reverse phase. Flow rate: 1.5mL/min.). Mass spectrum (ES+) m/z 202 (M + H).

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 22483-09-6.

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. 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 7252-83-7

A solution of 6-chloro-1,2-diazinan-3-amine (10 g, 73.75 mmol, l.OOequiv), 2-bromo-1,1-dimethoxyethane (50 g, 295.83 mmol, 4.01 equiv), and HBr(40%, 45 mL) in ethanol (100 mL) was stirred overnight at 90 C. The majority of the ethanol was removed under reduced pressure then the pH value of the solution was adjusted to 10 with 5% aqueous potassium carbonate solution. The resulting mixture was extracted with 6×500 mL of ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was purified on a silica gel column eluted with ethyl acetate/petroleum ether (1/2-1/1) to give 6,5 g (57%) of the title compound as a yellow solid. 1H NMR (300 MHz, CDCl3) delta 7.95 (s, 1 H), 7.91 (s, 1H), 7.80 (s, 1 H), 7.05 (d,.7 = 9.3 Hz, 1 H).

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 7252-83-7.

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. 70627-52-0, name is N-(4-(Benzyloxy)benzylidene)-4-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: N-(4-(Benzyloxy)benzylidene)-4-fluoroaniline

The raw material (III) (10 g, 28.0 mmol)And the starting material (IV) (17 g, 55.7 mmol)Was added to a 500 mL three-necked flask,Installed thermometer,Addition funnel and drying tube,Dry methylene chloride (150 mL) was added,The mixture was cooled to -20 C.Diisopropylethylamine (5.8 mL, 33.3 mmol) was added,Temperature control to -30 .Isopropyl titanate (3.0 mL, 10 mmol) was added,Maintaining the temperature at -25 C to -30 C,Titanium tetrachloride (3.3 mL, 30 mmol) was added dropwise.Control temperature <-25 ,The reaction was stirred for 5 hours,The reaction end point was detected by TLC.A mixed solution of slow acetic acid / dichloromethane (10 ml / 10 ml) was added to the reaction mixture,Drop add 2N sulfuric acid 30ml,The temperature was raised to 30 C for 30 minutes,Add water 30ml,Take the organic layer,The aqueous layer was extracted with 50 ml of dichloromethane,Combined organic layer,Followed by water 50ml,Saline 50ml washing,Dried over anhydrous sodium sulfate.After the solvent was distilled off,Add methanol 50ml,Reflux evenly,Standing slowly inside temperature 35 ,filter,The filter cake was washed with methanol 10 ml x 2,The solid was added to 50 ml of methanol,Reflux for 4 hours,Standing slowly cooled to the internal temperature of 40 ~ 45 ,filter,Filter cake with a small amount of methanol washing,Dried to a white solid (11.3 g, 17.1 mmol)Yield 60.9%. According to the analysis of related databases, 70627-52-0, the application of this compound in the production field has become more and more popular.

Synthetic Route of 51388-20-6, A common heterocyclic compound, 51388-20-6, name is 4-(Benzyloxy)aniline hydrochloride, molecular formula is C13H14ClNO, 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 XXV N-[4-(phenylmethoxy)phenyl]alanine ethyl ester A solution of 15 g (63.6 mmol) of 4-(phenylmethoxy)aniline hydrochloride in 200 ml of dimethylformamide is prepared and 13.8 g (76.4 mmol) of ethyl 2-bromopropionate are added, followed by 8.9 ml (63.6 mmol) of triethylamine. The reaction mixture is stirred for 24 h at 100 C. and then cooled and poured into 200 ml of iced water. The mixture is extracted with 2 times 200 ml of ethyl acetate and the combined organic phases are washed with water and then dried over sodium sulfate and concentrated under reduced pressure. The residue is purified by chromatography on silica gel using a cyclohexane/ethyl acetate mixture (95/5; v/v) as the eluent to give 10 g of the expected product in the form of an oil, which turns to beige crystals (yield=52%). M.p.=70 C.

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 19056-40-7, A common heterocyclic compound, 19056-40-7, name is 4-Bromo-3-methoxyaniline, molecular formula is C7H8BrNO, 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.

Step 1: 1 -(4-Bromo-3-methoxyphenyl)pyrrolidin-2-one Under an atmosphere of nitrogen, in a 100 mL round-bottomed flask at 0 °C, 4-bromo-3- methoxyaniline (2 g, 9.9 mmol) and KOH (6.93 ml, 13.9 mmol) were combined with dichloromethane (30 ml) to give a light brown solution. Then 4-bromobutanoyl chloride (1.84 g, 1.15 ml, 9.9 mmol) was added. The reaction was stined for 1 h at RT. The reaction mixture was poured into 50 ml dichioromethane and extracted with water (3 x 20 ml). The organic layer was dried over Na2SO4 and concentrated in vacuo.The residue was dissolved in 30m1 dichloromethane. Then tetrabutylammonium bromide (63.8 mg, 198 imol) and KOH (50 percent, 6 ml) were added. The reaction was stirred for 1 h at RT. The reaction mixture was poured into dichloromethane (50 ml) and extracted with water (3 x 20 ml).The organic layers were dried over Na2SO4 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 50 g, 20 percent to 50 percent EtOAc in heptane). The title compound was obtained as a off-white crystalline (1.92 g, 71.8 percent). MS (mle) = 272.1 [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.

Application of 6358-77-6, 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. 6358-77-6, name is 5-Bromo-2-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Preparation of (±)-12: A pressure glass tube charged with trifluoroborate (±)-10 (31 mg, 0.10 mmol), Cs2CO3 (98 mg, 0.30 mmol) and PdCl2(dppf)·CH2Cl2 (4 mg, 5 mol %) was alternatively evacuated and sparged with argon three times. A solution of 4-bromoanisol (21 mg, 0.11 mol) in toluene (1.5 mL) previously flushed with argon, then water (0.5 mL) were added by syringes. The reaction mixture was stirred at 100 C for 18 h and then cooled to room temperature. Water (5 mL) was added and the mixture extracted with EtOAc (5 mL × 2). The combined organic layers were washed with water (5 mL × 2), dried (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography (cyclohexane/EtOAc 9:1), affording 12 as a colorless oil (24 mg, 75%).

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

Reference of 104197-14-0,Some common heterocyclic compound, 104197-14-0, name is 4-Bromo-2,6-difluoroanisole, molecular formula is C7H5BrF2O, 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 136 Preparation of 1-(3,5-Difluoro-4-methoxyphenyl)-2,2,2-trifluoroethanone Isopropyl magnesium chloride lithium chloride complex (22.0 mL, 28.02 mmol) was added dropwise to a stirred solution of 5-bromo-1,3-difluoro-2-methoxybenzene (5.0 g, 22.42 mmol) at -5 C. in THF (100 mL) and the reaction mixture was stirred at same temperature for 30 min. Methyl triflouroacetate (3.67 g, 28.69 mmol) was added dropwise and then the reaction mixture was stirred at ambient temperature for 2 h. A 2 N HCl solution (200 mL) was added to quench the reaction and then it was extracted with diethylether. The organic combinded layers were washed with brine dried (Na2SO4), filtered and concentrated to afford the title compound (5.4 g, crude) as a yellow liquid. The material was taken on to next step without further purification. 1H NMR (400 MHz, CDCl3) delta 7.68-7.60 (m, 2H), 4.19 (s, 3H); ESIMS m/z 240.1 ([M]+).

The synthetic route of 104197-14-0 has been constantly updated, and we look forward to future research findings.