Category: ethers-buliding-blocks

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 592-55-2 as follows. Recommanded Product: 1-Bromo-2-ethoxyethane

In a similar manner 1d was obtained from sodium (diglyme)2 3,4,5-triphenyl-1,2-diphosphacyclopentadienide (0.94 g, 1.52 mmol) and 1-bromo-2-ethoxyethane BrCH2CH2OEt (0.26 g, 1.90 mmol, 25% excess) as a light-yellow oil; yield 0.36 g (59%). 1H NMR (CDCl3): 0.59 (t, 3H, 3JHH = 6.9, 3), 1.42-1.47 (m, 2H, OCH2), 1.51-1.57 (m, 2H, OCH2), 1.88-1.93 (m, 2H, PCH2), 6.85 (d, 4H, 3JHH = 3.42), 6.90 (d, 2H, 3JHH = 7.34), 6.96 (d, 4H, 3JHH = 6.85), 6.99-7.07 (m, 1H, 3JHH = 5.38), 7.20 (d, 2H, 3JHH = 7.34), 7.29 (d, 2H, 3JHH = 5.87). 31P NMR (CDCl3): 51.9 (d, 1JPP = 407.3), 214.1 (d, 1JPP = 407.3). 13 NMR (CDCl3): 16.7 (s, CH3), 25.6 (s, CH2), 27.3 (d, 2JCP = 9.7, CH2), 37.8 (dd, 1JCP = 16.3, 2JCP = 5.8, CH2), 126.4 (s, p-Ph), 126.5 (s, p-Ph), 126.8 (s, p-Ph), 127.4 (s, m-Ph), 128.2 (s, m-Ph), 128.3 (s, m-Ph), 128.5 (s, o-Ph), 129.2 (s, o-Ph), 130.5 (d, 3JCP = 1.4, o-Ph), 131.7 (s, o-Ph), 133.5 (s, o-Ph), 137.6 (d, 3JCP = 6.2, ipso-Ph), 138.24 (dd, 3JCP = 10.4, 3JCP = 3.8, ipso-Ph), 142.8 (d, 3JCP = 9.8, ipso-Ph), 149.7 (ps.tr, 3JCP = 15.51, C4), 164.5 (dd, 1JCP = 7.3, 2JCP = 3.1, C5), 185.8 (dd, 1JCP = 47.1, 2JCP = 14.9, C3).

According to the analysis of related databases, 592-55-2, the application of this compound in the production field has become more and more popular.

Electric Literature of 102-52-3, A common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, molecular formula is C7H16O4, 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.

To a suspension of intermediate lId (1.834 g, 8.94 mmol) in EtOH (30 ml) were added malonaldehyde bis(dimethyl acetal) (1.63 ml, 9.84 mmol) and conc.HC1 (1 ml). The reaction mixture was stilTed at 70C for 2 hours. The cooled mixture was evaporated todryness, diluted saturated solution of NaHCO3 and extracted with EtOAc twice. The combined organics were washed with water, with saturated solution of NaC1, dried over MgSO4, filtered and evaporated. The final product was purified by silica gel chromatography using 0 to 30 % EtOAc/cyclohexane as eluent to give intermediate lie(1.380 g, 64%). ?H NMR (500 MHz, CDC13) oe 8.12 (d, J= 2.1 Hz, 1H), 7.94 (s, 1H), 7.85 (d, J= 8.3 Hz, 1H), 7.72 (d, J= 1.4 Hz, 1H), 7.40 (s, 1H), 7.36 (dd, J= 8.3, 1.8 Hz, 1H),7.32 (d, J= 1.7 Hz, 1H), 6.46-6.43 (m, 1H), 3.97 (s, 3H).

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.

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. 450-88-4, name is 1-Bromo-4-fluoro-2-methoxybenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-fluoro-2-methoxybenzene

A mixture of 1 -bromo-4-fluoro-2-methoxybenzene (CAS No. [450-88-4]; 10.0 g, 48.8 mmol) in concentrated sulfuric acid (50 mL) was cooled to 0 C and treated dropwise with a freshly prepared mixture of fuming nitric acid (1.05 eq., 2.1 mL, 51 mmol) and concentrated sulfuric acid (1.85 eq., 4.8 mL, 90 mmol). The reaction mixture was stirred at 0 C for 30 minutes and poured in small portions on ice water. The formed precipitate was filtered off, washed with cold water and kept. The filtrate was extracted with ethyl acetate and the organic layer combined with the isolated precipitation. The organic layer was dried with sodium sulfate and concentrated in vacuo. The obtained material was purified by flash chromatography (SiO2-hexane/ ethyl acetate) to give the title compound (5.88 g, 44%). (0555) 1H-NMR (400MHz, DMSO-d6): [ppm] = 4.00 (s, 3H), 7.44 (d, 1 H), 8.40 (d, 1 H).UPLC- MS (ESI-): [M – H]- = 248/250; Rt = 1.17 min (Br isotope pattern; Method E).

The synthetic route of 450-88-4 has been constantly updated, and we look forward to future research findings.

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.

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.

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.

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.

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.

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. 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.