Month: May 2021

Related Products of 111-95-5,Some common heterocyclic compound, 111-95-5, name is Bis(2-methoxyethyl)amine, molecular formula is C6H15NO2, 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 following reactions were carried out in an argon gas atmosphere. There was dissolved, in toluene (3 mL), 2-(4-bromo-phenyl)-5-chloro-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine (59.0 mg, 0.150 mM), there were then added, to the solution, a solution of sodium t-butoxide (21.6 mg, 0.225 mM), tris(dibenzylidene acetone) di-palladium (6.9 mg, 0.0076 mM) and tri-t-butyl phosphine (10.9 muL, 0.0453 mM) in toluene (0.556 mL) and bis-(2-methoxyethyl)-amine (33.2 muL, 0.225 mM) and the resulting mixture was stirred at 80 C. for 4 hours and a half. This reaction liquid was diluted with a saturated aqueous common salt solution and then extracted with ethyl acetate. The extracts thus obtained were combined, dried over anhydrous sodium sulfate, then the solvent was distilled off and the resulting residue was purified by the silica gel column chromatography (ethyl acetate//hexane=1:4 to 2:3) to thus give the title compound (42.0 mg, yield: 63%). 1H-NMR (300 MHz, CDCl3): delta 3.37 (2s each 3H), 3.55-3.64 (m, 8H), 3.83-3.86 (m, 4H), 3.97-4.00 (m, 4H), 6.10 (s, 1H), 6.65 (s, 1H), 6.78 (d, 2H, J=8.5 Hz), 7.79 (d, 2H, J=8.5 Hz); MS (ESI) m/z 446 (M+H)+.

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

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 162705-07-9 as follows. Computed Properties of C18H21NO4

General procedure: To a solution of substituted benzyl-1H-1,2,3-triazole-4-carboxylic acids (18a-e, 1 mmol) in dry dimethylformamide, EDCI (1.2 mmol) and HOBT (1.2 mmol) were added and the reaction mixture was stirred for 20 min. To the reaction mixture, amino Z-stilbenes (16, 17, 1 mmol) was added and stirred at room temperature for 12 h. The solvent was removed and the residue was dissolved in dichloromethane (50 mL), washed with 5% HCl (2 20 mL), 5% NaHCO3 (2 20 mL), and brine solution (20 mL). The organic layer was separated, dried over anhydrous Na2SO4, filtered, and the solvent was removed to give a crude product which was purified by chromatography (ethyl acetate/hexanes) to givethe desired product (6a-e, 7a-e).

According to the analysis of related databases, 162705-07-9, the application of this compound in the production field has become more and more popular.

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., category: ethers-buliding-blocks

To a stirred solution of 1 -bromo-4-fluoro-2-methoxybenzene (4.0 g) in DMF (40 mL) was added sodium methanethiolate (2.76 g). The mixture was stirred at room temperature for 30 minutes and at 85 C for 2 h. Water was added and the mixture was extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution, dried (sodium sulfate) and the solvent was removed in vacuum. Silica gel chromatography gave 280 mg of the title compound.1H-NMR (400MHz, DMSO-d6): delta [ppm] = 2.46 (s, 3H), 3.82 (s, 3H), 6.74 (dd, 1 H), 6.91 (d, 1 H), 7.44 (d, 1 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.

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. 22171-15-9, name is (4-(Benzyloxy)phenyl)methanamine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 22171-15-9

Preparation Example A+-8. N-(4-Benzyloxy-benzyl)-6-(ethoxymethyl-amino)-nicotinamide To a solution of 6-aminonicotinic acid (130mg, 0.941 mmol) and 4-benzyloxy-benzylamine (201 mg, 0.941 mmol) described in Preparation Example 1 in N,N-dimethylformamide (5mL), was added benzotriazol-1-yl-tris(dimethylamino)phosphonium hexafluorophosphate (624mg, 1.41mmol) and triethylamine (394mul, 2.82mmol), and the solution was stirred for 40 minutes at 80C. Water and ethyl acetate were added to the reaction solution, which was then partitioned, and the organic layer was washed twice with water. The solvent was evaporated in vacuo, ethyl acetate was added to the residue, a white insoluble matter was collected by filtration, and 6-amino-N-(4-benzyloxy-benzyl)-nicotinamide (202mg, 0.606mmol, 64%) was obtained. To a solution of the resulting 6-amino-N-(4-benzyloxy-benzyl)-nicotinamide (200mg, 0.556mmol) in ethanol (10mL) were added 5,5-dimethylimidazophospho-2,4-dione (85mg, 0.66mmol) and 37% formaldehyde aqueous solution (1mL), and the solution was stirred for 1 hour under reflux. Water and ethyl acetate were added to the reaction solution, which was then partitioned, and the organic layer was washed twice. NH silica gel was added to the organic layer, the solvent was evaporated in vacuo for adsorption, purification was carried out by NH silica gel column chromatography (ethyl acetate), and the title compound (95mg, 0.243mmol, 40%) was obtained as a white solid. 1H-NMR Spectrum (CDCl3) delta (ppm) :1.20 (3H, t, J=7.0Hz), 3.55 (2H, q, J=7.0Hz), 4.56 (2H, d, J=5.5Hz), 4.84 (2H, s), 5.07 (2H, s), 5.68 (1 H, brs), 6.14 (1 H, brs), 6.62 (1 H, d, J=8.8Hz), 6.96 (2H, d, J=8.8Hz), 7.22-7.35 (4H, m), 7.27-7.44 (3H, m), 7.93 (1 H, dd, J=2.4, 8.8Hz), 8.54 (1 H, d, J=2.4Hz).

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 22171-15-9.

Reference of 910251-11-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 910251-11-5 name is Potassium trifluoro(methoxymethyl)borate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A vessel was charged with 4-[[2-(3-bromophenyl)acetyljaminoj-N-tert-butyl-pyridine-2- carboxamide (Example 54 step 1)(50 mg, 0.13 mmol) PdCl2dppf (3 mg), potassium trifluoro(methoxymethyl)boranuide (0.45 mL, 0.26 mmol) 2M aq. sodium carbonate (0.26mL, 0.51 mmol) and heated at8O Cfor 16 hours. The mixture was allowed to cool to room temperature, poured onto water (20 mL) and extracted into EtOAc (3 x 20 mL). The combined organic extracts were washed with brine (50 mL), dried over Na2504 and concentrated in vacuo. The residue was dissolved in DMSO:MeCN (800 p1, 1:1), filtered and purified by preparative HPLC (acidic pH, early elution method) to afford the titledcompound as an off-white solid.1H NMR (500 MHz, DMSO-d6) O 10.76 (5, 1H), 8.44 (d, J = 5.5 Hz, 1H), 8.18 (d, J = 2.1Hz, 1H), 8.02 (5, 1H), 7.81 (dd, J = 5.5, 2.2 Hz, 1H), 7.34-7.27 (m, 2H), 7.25 (d, J = 7.7Hz, 1H), 7.20 (d, J = 7.5 Hz, 1H), 4.40 (5, 2H), 3.71 (5, 2H), 3.29 (5, 3H), 1.39 (5, 9H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Potassium trifluoro(methoxymethyl)borate, and friends who are interested can also refer to it.

Related Products of 1758-46-9,Some common heterocyclic compound, 1758-46-9, name is 2-Phenoxyethylamine, molecular formula is C8H11NO, 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 2, 6-dichloronicotinic acid (960 mg, 5 mmol) in toluene (9 mL) was added SOC12 (547 mL, 7.5 mmol) and 2 drops of DMF. The mixture was heated at 90°C for 2 h, then cooled to room temperature. The solvent was removed in vacuo and the residual yellow oil was dried under high vacuum overnight. The residue was dissolved in anhydrous THF (20 mL) and cooled TO-78°C. Triethylamine (2.1 mL, 15 mmol) and 2-phenoxyethylamine (653 PL, 5 mmol) were added, and the reaction was stirred for 1.5 H, then quenched by pouring into a mixture of saturated NAHC03 and CH2C12. The aqueous layer was extracted with CH2C12. The organic extracts were combined and dried (MGS04), then concentrated to give a yellow oil, which was purified by flash chromatography on silica gel eluting with 35percent EtOAc/hexane to give the amide as a white solid (1.78 g, 82percent). MS (ES+) m/z (M+H) += 311. 16. 1H NMR (400 MHz, CDC13) : 8 3.87-3. 91 (m, 2H), 4.17 (t, J = 5.21 Hz, 2H), 6.90-7. 04 (m, 4H), 7.26-7. 32 (m, 2H), 7.36 (d, J = 8.05 Hz, 1H), 8.09 (d, J = 8. 05 Hz, 1H). HPLC : Retention time = 2.91 min (Method A).

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

Electric Literature of 162705-07-9,Some common heterocyclic compound, 162705-07-9, name is (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, molecular formula is C18H21NO4, 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.

3′ CA4-amine (0.11 g, 0.35 mmol) was dissolved in CH2Cl2 (10 mL), and then Fmoc-serine acetate (0.19 g, 0.52 mmol), T3P (0.62 mL, 1.0 mmol), and Et3N (0.073 mL, 0.52 mmol) were added. After stirring for 16 h at room temperature, water (10 mL) was added, and the reactionS3mixture was extracted with CH2Cl2 (3 × 10 mL). The combined organic phase was rinsed with brine, dried with Na2SO4, and concentrated under reduced pressure, and the residue was purified by flash column chromatography using a pre-packed 10 g silica column [solvent A: EtOAc; solvent B: hexanes; gradient: 12%A / 88%B (1 CV), 12%A / 88%B ? 100%A / 0%B (10 CV), 100%A / 0%B (2 CV); flow rate: 36 mL/min; monitored at 254 and 280 nm] affording the desired Fmoc-L-serinamide acetate 47 (0.22 g, 0.32 mmol, 93%) as a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, its application will become more common.

Electric Literature of 7664-66-6, A common heterocyclic compound, 7664-66-6, name is 4-Isopropoxyaniline, molecular formula is C9H13NO, 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.

4-Isopropoxy-phenylamine (11.3 g) was added to a solution of 4-hydroxy-l-(2-methoxy- ethyl)-cyclohexanecarboxylic acid ethyl ester (11.5 g) in toluene (361 ml). The mixture was stirred for 10 minutes at RT. Then, dimethylaluminiumchloride (0.9 M in hexane, 99 ml) was added dropwise and the reaction mixture was heated to reflux for 4 h. The mixture was then cooled to 0C, water (50 ml) was added dropwise then AcOEt (300 ml). The mixture was stirred further 30 minutes, more AcOEt was added, the layers were then separated, the organic layer was dried over MgS04, filtered and the solvent was evaporated off . The crude product was triturated with diethyl ether/heptane to give the title compound as a mixture of cis/trans isomers as brown solid (14.3 g) which was used directly in the next step. MS (m/e): 304.190 [MH+].

The synthetic route of 7664-66-6 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 1663-61-2, name is (Triethoxymethyl)benzene, 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. category: ethers-buliding-blocks

General procedure: The starting hydrazide 4, 8e-i (10 mmol) was added to a mixture of the appropriate triethyl orthoester (10 mol) and 0.1 g p-TsOH in 20 mL of xylene and kept under reflux for 3 h (TLC). After cooling, the mixture was washed with water (30 mL), dried over MgSO4 and then concentrated under reduced pressure. The oily residue was subjected to column chromatography (silica gel, eluent: hexane/AcOEt, 1:2 v/v) or crystallised from benzene/hexane mixture.

The synthetic route of (Triethoxymethyl)benzene has been constantly updated, and we look forward to future research findings.

Electric Literature of 39538-68-6, 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 39538-68-6 as follows.

5.2 g of 2-methoxy-4-methylaniline was dissolved in 32 ml of water and 11.4 ml of concentrated hydrochloricacid, cooled to 0-5 C in an ice bath, and 2.88 g of sodium nitrite dissolved in 9 ml of water was added dropwise to theabove cooled solution. The mixture was stirred for 10 minutes in an ice bath and then 5.6 g of sodium acetate was added.The above reaction liquid was added dropwise to a hot (about 75 C) solution wherein 11 g of potassium ethyl xanthatewas dissolved in 51 ml of water, stirred for another 1 hour, cooled to room temperature, and extracted with ethyl acetate.After liquid separation, the organic phase was washed with saturated aqueous solution of sodium chloride and thendried over anhydrous sodium sulfate, filtered, concentrated, and then dissolved in a solution of 1.3 N potassium hydroxidein ethanol, and then added with 3 g of glucose and refluxed for 3 hours. The reaction mixture was concentrated and thepH was adjusted to about 1 with 6 N sulfuric acid in ice bath, and then 5.7 g of zinc powder was added and heated andstirred at 50 C for 30 minutes. The insoluble was filtered off and the filtrate was extracted with ethyl acetate. After liquidseparation, the organic phase was washed with saturated aqueous solution of sodium chloride and dried over anhydroussodium sulfate, filtered and concentrated, and the residue was separated by column chromatography (100% petroleumether) to afford 4.15 g of oily matter, yield 71%.1H NMR (300 MHz, DMSO-d6) delta 7.17 (s, 1H), 6.81 (s, 1H), 6.66 (s, 1H), 4.63 (s, 1H), 3.80 (s, 3H), 2.26 (s, 3H).

According to the analysis of related databases, 39538-68-6, the application of this compound in the production field has become more and more popular.