Category: ethers-buliding-blocks

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. 3616-56-6, name is 2,2-Diethoxy-N,N-dimethylethanamine, A new synthetic method of this compound is introduced below., Recommanded Product: 2,2-Diethoxy-N,N-dimethylethanamine

The mixture of homocoupling product 2i (0.5 mmol), NaOEt (340.25 mg, 5.0 mmol) and DMSO (1.0 mL) was added into a 35 ml pressure-resistant vial under air atmosphere. The mixture was heated to 120oC and stirred for 5h. After being cooled to ambient temperature, the reaction mixture was diluted with EtOAc (60 mL) and washed with H2O (2×30 mL). The aqueous phase was extracted with EtOAc (2×30 mL), and the combined organic phase was dried over anhydrous Na2SO4, filtered and concentrated under the reduced pressure. The residue was purified by silica gel column directly to give the product 3i (Yield 82%). The spectra of 3i were in accordance with those reported in the literature3. Then 16.1mg (1.0 mmol) (dimethylamino)acetaldehyde diethyl acetal was added in the refluxing mixture of 30 mg (0.10 mmol) biindole 3i with the 3ml of AcOH solvent. The resulting mixture was refluxed for 2 h, then cooled to room temperature, and concentrated under reduced pressure. The residue was purified by silica gel chromatography to give tjipanazole D (4i) with 65% yield (21.1 mg). The spectra of 4i were in accordance with those reported in the literature3,4,5.

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 126-38-5,Some common heterocyclic compound, 126-38-5, name is 1-Bromo-2,2-dimethoxypropane, molecular formula is C5H11BrO2, 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.

The compound 4,6-dimethoxypyrimidine-5-carboxamide (500 mg, 2.73 mmol) was suspended in1-bromo-2,2-dimethoxypropane (5 mL),The mixture was heated to 130 C and stirred for 1.5 hours. The reaction was monitored by thin-layer chromatography (PE / EtOAc, v / v, 2/1). After the reaction was completed, the reaction mixture was diluted with ethyl acetate (30 mL). The resulting mixture was washed with water (30 mL) and brine (30 mL), and the organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (PE / EtOAc (v / v) = 8/1) to give the title compound as a white solid (229 mg, 37.9%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,2-dimethoxypropane, its application will become more common.

Related Products of 1978-39-8,Some common heterocyclic compound, 1978-39-8, name is 5-Fluoro-2-methoxyaniline, molecular formula is C7H8FNO, 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 2 (5) obtained in 2 – [[5- (4-hydroxy-3-methoxyphenyl)-4-(lH-pyrrol-1-yl)-4H-1,2,4-triazole -3 – yl] thio] acetic acid (200mg, 0.58mmol),1-hydroxybenzotriazole (80mg, 0.6mmol),1-ethyl-3- (3-dimethylaminopropyl) carbodiimide hydrochloride (120 mg, 0.6 mmol)Of N, N-dimethylformamide (4 ml)Was added triethylamine (0.18ml, 1.2mmol)When the 5-fluoro-2-methoxy aniline (0.08ml, 0.7mmol)Was stirred for 16 hours at room temperature added.It was extracted by the addition of 1N hydrochloric acid and ethyl acetate to the reaction solution. Further, the aqueous layer was extracted twice with ethyl acetate, the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, the residue was purified by column (hexane: ethyl acetate = 1: 3-1: 5) to give N-(5-fluoro-2-methoxyphenyl) -2 – [[5- ( 4-hydroxy-3-methoxyphenyl) -4- (1H- pyrrol-1-yl) -4H-1,2,4- triazol-3-yl] thio] acetamide (30mg, 11%) a pale brown solid It was obtained as a.

The synthetic route of 1978-39-8 has been constantly updated, and we look forward to future research findings.

Application of 446-59-3, A common heterocyclic compound, 446-59-3, name is 2-Bromo-1-fluoro-3-methoxybenzene, molecular formula is C7H6BrFO, 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.

Intermediate 1-40fluoro-phenol (1-40)To a solution of 2-bromo-3-fluoroanisole [C.A.S. 935285-66-8] (1 g, 4.48) in DCM (2 mL), BBr3 (17.93 mL, 17.93 mmol) was added dropwise at 0C. The reaction was stirred 2 h at r.t. Then the excess of BBr3 was quenched dropwise with water at 0C, the organic layer was separated, dried (Na2S04), filtered and the solvent evaporated in vacuo to yield intermediate 1-40 (0.94 g, quant, yield) that was used as such in the next reaction step

The synthetic route of 446-59-3 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. 588-96-5, name is p-Bromophenetole, A new synthetic method of this compound is introduced below., name: p-Bromophenetole

(3) Dissolve 1 g of p-bromophenylethyl ether in 30 mL of 1,4-dioxane solution, add 1.2 equivalents of bis(pinacolato)diboron, 3 equivalents of potassium acetate, 5% equivalent of [1,1′-double (Diphenylphosphino)ferrocene]palladium dichloride was subjected to argon gas treatment at 80 C for 8 hours, and the product was obtained by column chromatography.

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. 95970-05-1, name is 2,6-Dibromo-4-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows., category: ethers-buliding-blocks

A 250 mL round bottom flask equipped with a stir bar, Vigreux column and nitrogen inlet was charged with 2,6-dibromo-4-methoxy-phenylamine, (14 g, 50 mmol) and NMP, (80 mL). Copper cyanide, (18 g, 200 mmol) was then added at ambient temperature and the reaction was heated at 140 C oil bath temperature. The reaction was allowed left to stir for 24 h. The reaction was cooled, diluted with EtOAc, (1000 mL) and poured into 1000 mL of 10% ethylene diamine solution. The mixture was stirred vigorously for 2 h. The mixture was filtered through a pad of celite and washed with copious EtOAc (poor solubility) and the phases were split. The aqueous phase was extracted with EtOAc, (500 mL) (chi3), the combined EtOAc extracts were washed with water (500 mL), dried (Na2SO4), and the solvent was evaporated under reduced pressure. The material was passed through a pad of silica gel eluting with DCM-EtOAc (10% EtOAc). Amount obtained: 5.0 g, 29 mmol, 58% yield.

According to the analysis of related databases, 95970-05-1, 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. 92248-06-1, name is Bis(3-methoxyphenyl)amine, This compound has unique chemical properties. The synthetic route is as follows., category: ethers-buliding-blocks

To a solution of bis(3-methoxyphenyl)amine (1.15g, 5.00mmol) in THF (20mL) at RT was added sodium hydride (60% dispersion in mineral oil, 550mg, 13.8mmol). The suspension was heated to 75C and stirred for 30 min at this temperature. Iodomethane (0.716mL, 11.5mmol) was added within 5 min at 75C and the reaction mixture was continued to stir for 2 h at this temperature. The suspension was treated with water (20mL) and extracted with Et2O (3×65mL). The combined organic layer was dried over Na2SO4 and concentrated in vacuo. Column chromatography on silica gel with pentane:CH2Cl2 3:1 to 1:1 gave 3-methoxy-N-(3-methoxyphenyl)-N-methylaniline (1d) as a yellowish oil (979mg, 81%): Rf 0.64 (CH2Cl2 100%); numax (neat): 2938w, 2834w, 2338w, 1589s, 1489s, 1347w, 1279w, 1221m, 1169w, 1122w, 1046w, 766s, 708w, 631s; 1H NMR (500MHz, CDCl3) delta=7.15-7.19 (2H, m, C5H), 6.62 (2H, ddd, 3J 8.1, 4J 2.2, 0.8, C6H), 6.57-6.58 (2H, m, C2H), 6.52 (2H, ddd, 3J 8.2, 4J 2.5, 0.8, C4H), 3.76 (6H, s, OCH3), 3.29 (3H, s, NCH3); 13C NMR (125MHz, CDCl3) delta=160.5 (C3), 150.2 (C1), 129.8 (C5), 113.3 (C6), 106.7 (C4), 106.6 (C2), 55.2 (OCH3), 40.3 (NCH3); ESI-MS: m/z calcd. for C15H18NO2+ 244.1332 found 244.1330 [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 92248-06-1.

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. 707-07-3, name is (Trimethoxymethyl)benzene, A new synthetic method of this compound is introduced below., Formula: C10H14O3

General procedure: To a stirred solution of the respective N-carbamate protected aminoalcohol 1 (0.50 mmol, 1 equiv) in CH2Cl2 (10 mL, 0.05 M) were added BF3·OEt2 (50 muL, 0.050 mmol, 0.1 equiv or 150 muL, 0.15 mmol, 3 equiv, 1.0 M solution in CH2Cl2) and trimethyl orthobenzoate (0.13 mL, 0.75 mmol, 1.5 equiv) at r.t. The resulting mixture was stirred at r.t. under N2 until TLC showed complete conversion of the substrate. The reaction was quenched with sat. aq NaHCO3 and extracted with EtOAc(2 ×). The combined organic layers were washed with brine, dried(MgSO4), filtered, and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (hexane/EtOAc) to give the desired product 2.

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 262587-05-3, 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 262587-05-3 as follows.

A nitrogen-purged mixture of tris(dibenzylideneacetone)dipalladium(0) (0.0193 g, 0.021 mmol), and di-tert-butyl(2′,4′,6′-triisopropyl-3,4,5,6-tetramethyl-[1,1′-biphenyl]-2-yl)phosphine (0.0251 g, 0.052 mmol) in toluene (2.2 mL) was stirred for 20 minutes and then added to an nitrogen-purged mixture of methyl 3-cyclobutyl-4-[4-(morpholin-4-yl)piperidin-1-yl]-1H-pyrazolo[3,4-b]pyridine-6-carboxylate (0.1760 g, 0.441 mmol, E509), 1-bromo-3-(difluoromethoxy)benzene (0.1179 g, 0.529 mmol), and Cs2CO3 (0.2143 g, 0.658 mmol). The mixture was heated to 70 C overnight, diluted with water, extracted with DCM (3 x 8 mL), dried (Na2SO4), and concentrated. The residue was chromatographed on silica (30-60% EtOAc/DCM to 4% MeOH/DCM) and re-chromatographed (2.5-4% zPrOH/DCM) to give the titled compound. 1H NMR (400 MHz, DMSO-d6) delta ppm 8.28 – 8.16 (m, 2H), 7.58 (t, J = 8.2 Hz, 1H), 7.51 – 7.03 (m, 3H), 3.95 (dq, J = 18.1, 9.8, 8.5 Hz, 1H), 3.88 (s, 3H), 3.63 – 3.48 (m, 6H), 2.91 (t, J = 11.9 Hz, 2H), 2.53 – 2.48 (m, 4H), 2.46 – 2.28 (m, 2H), 2.12 – 1.88 (m, 4H), 1.63 (td, J = 13.1, 12.6, 6.4 Hz, 2H).

According to the analysis of related databases, 262587-05-3, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 768-70-7, name is 3-Ethynylanisole, belongs to ethers-buliding-blocks 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 768-70-7, Computed Properties of C9H8O

General procedure: A mixture of CuII(BAPTE)Cl2-[n-Bu4N]4[Mo6O18]2 (1mol%, 30mg) in H2O/DMSO (3mL, 1:10) was stirred for 10min. Then, the phenylacetylenes (1.3mmol), benzyl halide (1mmol), sodium azide (1.1mmol) and sodium ascorbate (5mol%) were added, and the resulting mixture was stirred at room temperature. The progress of the reaction was monitored by TLC (eluting with n-hexane/ethyl acetate, 1:1). At the end of the reaction, methanol (5mL) was added to precipitate the catalyst. The catalyst was recovered by centrifugation, washed with methanol and diethyl ether, and dried in vaccuo. The filtrates were concentrated and the pure product was obtained by thin layer chromatography.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Ethynylanisole, and friends who are interested can also refer to it.