Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 111-95-5, name is Bis(2-methoxyethyl)amine, 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 111-95-5, name: Bis(2-methoxyethyl)amine

EXAMPLE 29 Bis-(2-methoxy-ethyl)-prop-2-ynyl-amine Propargyl bromide (17.8 g, 150 mmol) was added dropwise to a mixture of bis(2-methoxy-ethyl)amine (20 g, 150 mmol) and cesium carbonate (49 g, 150 mmol) in 350 mL of acetone. The mixture was stirred overnight under nitrogen at room temperature. The inorganic salts were then filtered off, and the solvent was removed. The residue was dissolved in saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic extracts were then evaporated to give 20 g of bis-(2-methoxy-ethyl)-prop-2-ynyl-amine: mass spectrum (m/e): M+H 172.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Bis(2-methoxyethyl)amine, and friends who are interested can also refer to it.

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. 7664-66-6, name is 4-Isopropoxyaniline, A new synthetic method of this compound is introduced below., category: ethers-buliding-blocks

[Example 1] Preparation of 1-(4-chlorobenzyl)-3-ethylamino-6-(4-isopropoxyphenylamino)benzene (I-071) To a mixture of 3-bromo-4-fluoro-1-nitrobenzene (1.0 g, 4.6 mmol) and DMSO (5 mL) were added potassium carbonate (1.01 mg, 7.3 mmol) and 4-isopropoxyaniline (1.03 g, 6.8 mmol), and the resulting mixture was stirred at 100C for 0.5 hours. To the reaction mixture was added water (20 mL), and the resulting mixture was extracted with ethyl acetate (30 mL*2). The extract was washed by brine (20 mL) and water, and the organic layer was dried over anhydrous sodium sulphate, and concentrated in vacuo. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane). The resulting residue was precipitated by ethyl acetate and hexane to give 3-bromo-4-(4-isopropoxyphenylamino)-1-nitrobenzene (0.55 g, Yield: 35%)as orange solid. 1H-NMR (delta ppm TMS/DMSO-d6): 1.28 (6H, d, J = 6.0 Hz), 4.61 (1H, sept, J= 6.0 Hz), 6.76 (1H, d, J = 9.0 Hz), 6.97 (2H, d, J = 9.0 Hz), 7.19 (2H, d, J = 9.0 Hz), 8.00 (1H, dd, J = 8.9 Hz, 2.4 Hz), 8.34 (2H, d, J = 2.4 Hz).

The synthetic route of 7664-66-6 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.

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.

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.

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 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.

Adding a certain compound to certain chemical reactions, such as: 321-28-8, name is 1-Fluoro-2-methoxybenzene, 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 321-28-8, name: 1-Fluoro-2-methoxybenzene

A stirred solution of 2-fluoroanisole (33.7 mL, 301 MMOL) in chloroform (250 mL) was cooled to 0C and treated drop-wise with chlorosulfonic acid (50.0 mL, 752 MMOL). After stirring at room temperature for 14 hours, the reaction mixture was poured into ice-water (700 mL) and the separated, aqueous phase extracted with chloroform (2 x 200 mL). The combined organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated IN VACUO TO YIELD 3-FLUORO-4- METHOXYBENZENESULFONYL CHLORIDE as a fine, white solid (58.6 g, 87%), m. p. 80C ; 1H NMR (400 MHz, DMSO-d6) 5 : 7.32 (m, 1H), 7.25 (dd, J= 11.5, 2.0 Hz, 1H), 7.05 (t, J = 8. 5 HZ, 1 H), 3.78 (s, 3H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Synthetic Route of 1579-40-4, 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. 1579-40-4, name is Di-p-tolyl Ether, This compound has unique chemical properties. The synthetic route is as follows.

20 g (0.1 mol) of 4,4′-dimethyl diphenyl ether,60 g of carbon tetrachloride and 0.82 g (0.005 mol) of azoisobutyronitrile were charged into the above four-necked flask,Heating the material through a water bath,After heating to 80 C with stirring, 36.8 g (0.23 mol) of bromine was added dropwise,1.1h drop finished,After the drop-back reaction 3.0h.The reaction liquid obtained by the refluxing reaction was subjected to atmospheric distillation of carbon tetrachloride,The material was then cooled to 50 & lt; 0 &To the cooled mass was added 98.4 g (0.3 mol) of a 25% solution of sodium isopropoxide in isopropanol,35min drop finished,Heating reflux 3.0h,The isopropanol was then distilled off.The carbon tetrachloride vaporization was 54.8 g,After washing to neutral and dry after carbon tetrachloride 54.2g,The purity was 99.1% by gas chromatography analysis,The recovery was 90.3%.The amount of isopropanol distilled off was 67.1 g,The purity was 95.6% by gas chromatography,The recovery was 86.9%.Recovery of isopropyl alcohol by distillation and drying dehydration can be used for sodium isopropoxide system.100 mL of water was added to the above materials,Stirring 10min after standing phase,The oil phase was washed twice with the remaining water,Each wash water 50mL.The washed oil phase is first distilled off under normal pressure,And then under a pressure of 1 ~ 2mmHg vacuum distillation,To obtain 23.8 g of a crude product having a boiling point of 220 to 230 C / 1 to 2 mmHg.After the crude product is obtained, the crude product is subjected to vacuum distillation treatment in the present invention to obtain pure product. The product purity was 99.8% by gas chromatography. The yield was calculated to be 92.8%.

The chemical industry reduces the impact on the environment during synthesis Di-p-tolyl Ether. I believe this compound will play a more active role in future production and life.

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. 54149-17-6, name is 1-Bromo-2-(2-methoxyethoxy)ethane, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 54149-17-6

To a vial containing ethyl 1H-indazoie-3-carboxyiate (150 mg, 0.789 inmol) in C1-I3CN (3 mL), were added I -bromo-2-(2-methoxyethoxy)etharie (217 mg, 1.183 mniol) and Cs?C03 (385 mg, 1.183 mrnol). The vial was sealed and the mixture was stirred at 80C overnight. Afterwards, water was added, extracted with EtOAc, washed organic layer with 10% LiCI, brine, concentrated and the residue was purified by normal phase chromatography with the second peak to elute off column being the desired product (105mg, 40.5%). MS (ESI) m/?: 293.2 (M±HY?. ?H NMR (400MHz, CDCI3) 5 8.20 (dt, J::r8.2,1.0 Hz, IH), 7.63- 7.57(m, 1H), 7.42 (ddd, J=8.4, 7.0, 1.1 Hz, IH), 7.30 (ddd, J=8.1,7.0, 0.9 Hz, 1H), 4.67 (t, J=5.6 Hz, 2H), 4.53 (q, J:::73 Hz, 21-1), 3.97 (t, J:::57 Hz. 21-1),3.56 – 3.48 (rn, 2H). 343 – 337 (m, 2H), 3.28 (s, 31:1), 1.48 (t, J:::7.2 Hz,3H).

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 54149-17-6.