Month: May 2021

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.

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.

Related Products of 54149-17-6, 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. 54149-17-6 name is 1-Bromo-2-(2-methoxyethoxy)ethane, 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.

Under a nitrogen atmosphere, 2.00 g of the compound represented by the formula (C-7-1) and 20 mL of N,N-dimethylformamide were placed in a reaction vessel.While ice-cooling, 1.49 g of tertiary potassium butoxide was added, and the mixture was stirred at room temperature for 1 hour.While cooling with ice, a solution obtained by dissolving 2.44 g of the compound represented by the formula (C-7-2) in 3 mL of N,N-dimethylformamide was added dropwise.After stirring at room temperature for 5 hours, it was diluted with 100 mL of dichloromethane and poured into water.The organic layer was washed with brine and dried over sodium sulfate, and the solvent was evaporated.By subjecting column chromatography (alumina, dichloromethane) and recrystallization (dichloromethane/hexane), 3.04 g of the compound of formula (C-7) was obtained.The yield of the compound represented by the formula (C-7-1) was 94%.The reaction solution after the reaction showed a light coloration.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2-(2-methoxyethoxy)ethane, and friends who are interested can also refer to it.

Electric Literature of 4393-09-3,Some common heterocyclic compound, 4393-09-3, name is (2,3-Dimethoxyphenyl)methanamine, molecular formula is C9H13NO2, 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.

8-Chloro-2,2-dimethyl-5-(pyrrolidin-1 -yl)-1 ,4-dihydro-2/-/- pyrano[4″,3″:4l,5′]pyrido[3′,2′:4,5]thieno[3,2-c/]pyrimidine (O.Odeltag, 0.21 mmol, see Preparation 24) is suspended in ethanol (5 ml) and (2,3-dimethoxybenzyl)amine (0.16 ml, 1.07 mmol) is added. The mixture is refluxed for 24h and then allowed to cool to room temperature. The solvent is evaporated under vacuum and the residue is purified by chromatography, eluting first with CH2CI2 and then with CH2CI2:Me0H 99:1. 85 mg of the desired final product are obtained. Yield= 79%. m.p. 166.0-167.50C1 H NMR (300 MHz, DMSO-D6) delta ppm 1.32 (s,6 H) 1.88 (m, 4 H) 3.33 (d, J=7.02 Hz, 3 H) 3.60 (m, 4 H) 3.78 (m, 6 H) 4.74 (d, J=5.80 Hz, 2 H) 4.83 (s, 2 H) 6.83 (dd, J=7.17, 1.98 Hz, 1 H) 6.96 (m, 1 H) 8.01 (t, J=5.80 Hz, 1 H) 8.48 (s, 1 H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route (2,3-Dimethoxyphenyl)methanamine, 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 24878-25-9 as follows. Quality Control of 2,2′-Oxydianiline

A solution of 2-hydroxy-5-(thiophen-2-yl)benzaldehyde (3)(1.34 g, 2.0 mmol) in ethanol (30 mL) was added to a solution of2,20-oxydianiline (2-aminophenyl ether) (4) (0.66 g, 1.0 mmol) inethanol (20 mL) with continuous stirring, and the mixture wasrefluxed for 24 h. The completion of the reaction was monitoredthrough TLC. The reaction mixture was then cooled to room temperatureand ethanol was removed. The obtained residue waswashed with ethanol and dried at room temperature. The productwas recrystallized from the mixture of ethanol:kloroform (1:2). Theyield of orange product OPBTS was 46% (1.72 g), (m.p. 172-175 C).FTIR (KBr, cm-1) 3436.04 (nuO-H phenolic), 3268.00-3120.01 (nuAr C-H),1621.17 (nuCN), 1575.90e1489.00 (nuAr CC), 816.62 and 681.50 (nuC-SC).1H NMR (400 MHz, DMSO-d6) delta (ppm) 13.27 (s, 1H, ArO-H), 9.02(s, 1H, -CHN), 7.82 (d, 1H, J 2.4 Hz, Ar-H), 7.61 (dd, 1H, J 8.4,J 2.4 Hz, Ar-H), 7.55 (dd, 1H, J 7.4 Hz, J 1.8 Hz, Ar-H), 7.40 (dd,1H, J 5.2 Hz, J 1.2 Hz, Th-H), 7.30 (dd, 1H, J 3.6 Hz, J 1.2 Hz,Th-H), 7.26e7.23 (m, 2H, Ar-H), 7.04 (dd, 1H, J 5.2 Hz, J 3.6 Hz,Th-H), 6.94 (dd, 1H, J 8.0 Hz, J 1.6 Hz, Ar-H), 6.87 (d, 1H,J 8.8 Hz, Ar-H). 13C NMR (100 MHz, DMSO-d6) delta (ppm) 163.73,160.46,150.20,143.07,138.89,130.94,129.48,128.91,128.85,125.53,125.08, 123.03, 120.58, 119.82, 119.48, 117.92. Elemental anal. calcd.for C34H24N2O3S2: C, 71.31; H, 4.22; N, 4.89; O, 8.38; S,11.20%. FoundC, 70.86; H, 4.21; N, 4.90; S, 10.87%.

According to the analysis of related databases, 24878-25-9, the application of this compound in the production field has become more and more popular.

Related Products of 82830-49-7, The chemical industry reduces the impact on the environment during synthesis 82830-49-7, name is 2-Fluoro-1,4-dimethoxybenzene, I believe this compound will play a more active role in future production and life.

To a solution of 2-fluoro-1,4-dimethoxybenzene (2.56 g, 0.0 16 mol) in dry THF (100 mL) at -78 C was added n-BuLi (2.5 M, 7 mL, 0.0 17 mol) dropwise under a N2 atmosphere. The reaction was stuffed at -78 C for 1 h and then ethyl chloroformate (1.8 g, 0.0 17 mol) inTHF (50 mL) was added dropwise at -78 C. The reaction mixture was stirred at -78 C for another 1 h. The reaction was warmed slowly to room temperature and quenched with a saturated aqueous NH4C1 solution (100 mL). The reaction mixture was extracted with ethyl acetate (100 mL x 3). The combined organic phases were dried with MgSO4 and concentrated to afford the crude material which was purified by column chromatography on silica gel(petroleum ether/ethyl acetate 1:10 to 1:5) to afford pure methyl 2-fluoro-3,6- dimethoxybenzoate (2.28 g, 65% yield).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Fluoro-1,4-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Some common heterocyclic compound, 171290-52-1, name is 3,5-Dimethoxyphenylacetylene, molecular formula is C10H10O2, 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. Safety of 3,5-Dimethoxyphenylacetylene

General procedure: To a solution of an alkyne 2 (1.2 equiv) in anhydrous toluene (3 mL) under an argon atmosphere, KOtBu (1.0 equiv) was added, and the mixture was stirred for 10-15 min. Then, an N-protected isatin 1 (1.0 equiv) was added to the reaction mixture, which was stirred for 30 min to 3 h until all the isatin was consumed (confirmed by TLC). The reaction was finally quenched with a few drops of 1 N HCl and the resulting mixture was extracted with CH2Cl2 (2 × 15 mL). The combined organic phases were washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The crude residue was then purified by column chromatography on silica gel (EtOAc-hexane,10:90 to 30:70) to give compounds 3.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 171290-52-1, its application will become more common.

Electric Literature of 20781-20-8,Some common heterocyclic compound, 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, molecular formula is C9H13NO2, 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 solution of 2,4- dimethoxybenzaldehyde (Sigma-Aldrich, 5.00 g, 30.1 mmol) in MeOH (100 mL) was added 2,4-dimethoxybenzylamine (Sigma-Aldrich, 5.53 mL, 33.1 mmol). The resulting mixture was stirred at RT for 1 h and then sodium borohydride (1.30 g, 34.3 mmol) was added slowly. Gas evolution was observed. After stirring at RT overnight, the reaction was quenched with water and then partially concentrated to remove MeOH in vacuo. The residue was extracted with EtOAc (3X). The combined organic layers were washed with brine (1X), dried over anhydrous magnesium sulfate and concentrated in vacuo to afford 98.1 as a colorless oil. The product was used directly in the next step. LCMS-ESI (pos.) m/z: 318.2 (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 (2,4-Dimethoxyphenyl)methanamine, its application will become more common.

Application of 645-36-3, 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. 645-36-3 name is 2,2-Diethoxyethanamine, 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.

To a stirred solution of 2-bromo-5-(trifluoromethyl)benzoic acid (5 g, 18.59 mmol) in 50 mL DMF at 0 C was added HATU (10.60 g, 27.9 mmol) and triethylamine (3.89 ml, 27.9 mmol). The reaction mixture was stirred for 15 min. and then 2, 2-diethoxyethanamine (4.05 ml, 27.9 mmol) was added to it and the reaction mixture was slowly warmed to room temperature and stirred for 12 h. The reaction mixture was diluted with ice cold water, and the precipitate obtained was filtered and the residue was dissolved in ethyl acetate, dried over sodium sulphate and concentrated to get the product as white solid. (Yield = 6 g, 85%). NMR (400 MHz, Chloroform-if) delta 7.82 (d, J = 2.8 Hz, 1H), 7.76 (d, J = 8.3 Hz, 1H), 7.55 (d, J = 8.3 Hz, 1H), 6.33 (s, 1H), 4.69 (dd, J = 6.0, 3.6 Hz, 1H), 3.83 – 3.72 (m, 2H), 3.68 – 3.57 (m, 4H), 1.30 – 1.18 (m, 6H). LCMS (ESI) : m/z 406.07 & 408.07(M+Na)+

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,2-Diethoxyethanamine, 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. 1462-37-9, name is ((2-Bromoethoxy)methyl)benzene, A new synthetic method of this compound is introduced below., Product Details of 1462-37-9

To a solution of 4-hydroxy-3,5-dimethylbenzaldehyde (6.84 g, 0.0455 mol) in anhydrous DMF (15 mL) was added NaH in mineral oil (60percent, 2.23 g, 0.0558 mol). (2-Bromo-ethyoxymethyl)-benzene (10.0 g, 0.0465 mol) was added and the reaction was kept at 65° C. overnight. The reaction mixture was poured into water and extracted with dichloromethane to yield (4-(2-benzyloxy-ethoxy)-3,5-dimethylbenzaldehyde (10.5 g, 81percent), which was used for next step reaction without further purification

The synthetic route of 1462-37-9 has been constantly updated, and we look forward to future research findings.