Tag: M.W=100-200

Application of 52189-63-6, 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. 52189-63-6 name is 1-Fluoro-3,5-dimethoxybenzene, 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.

Step 4: Intermediate 5-f: To a solution of 1-fiuoro-3,5-dimethoxybenzene (12.5 g, 80 mmol) in dichloromethane (80 ml) cooled to 0C was added dropwise over a period of 30 minutes a 1.0 M solution of BBr3 in dichloromethane (200 ml, 200 mmol). The reaction was stirred for 1 hour at 0C and then slowly warmed to room temperature and stirred for 18 hours. The reaction was cooled to 0C and quenched by slow addition of MeOH and water. After stirring at room temperature for 1 hour the mixture was filtered and volatiles were removed under reduced pressure. Ethyl acetate was added to the residue; a precipitate formed and was collected by filtration to provide intermediate 5-f as orange solid

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Fluoro-3,5-dimethoxybenzene, and friends who are interested can also refer to it.

Reference:
Patent; PHARMASCIENCE, INC.; LAURENT, Alain; ROSE, Yannick; WO2014/29007; (2014); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 1579-40-4, The chemical industry reduces the impact on the environment during synthesis 1579-40-4, name is Di-p-tolyl Ether, I believe this compound will play a more active role in future production and life.

Prior to use, NBS was recrystallized from water and the carbon tetrachloride was bubbled with nitrogen, stirred for 45 min with sodium sulfate, and checked by 1H-NMR spectroscopy. To a stirred solution of 4,4′-oxybis(methylbenzene) (28) (5.0 g, 25.2 mmol, 1 eq.) and NBS (8.98 g, 50.4 mmol, 2 eq.) in carbon tetrachloride (125 mL) under nitrogen was added a catalytic amount of AIBN. The reaction mixture was heated to 80-90 C (reflux) and stirred for 6.5 h. The solution was then cooled and the succinimide was removed on a sintered glass filter funnel. The solvent was removed in vacuo to yield the desired product 29 as beige crystals (8.3 g, 93%). A portion (1.82 g) was purified by flash chromatography (10:1 hexane:EtOAc) to yield 29 as white crystals: mp 85-86 C (lit.29 mp 93-95 C). 1H NMR (CDCl3): delta 7.38 (d, 4H), 6.98 (d, 4H), 4.52 (s, 4H).

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, Di-p-tolyl Ether, other downstream synthetic routes, hurry up and to see.

Reference:
Article; McGowan, Meredeth A.; Perreault, Denise M.; Thornton, Nancy B.; Garaas, Sarah D.; Gribble, Gordon W.; Arkivoc; vol. 2018; 5; (2018); p. 334 – 347;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Synthetic Route of 37466-89-0, 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. 37466-89-0 name is 3-Methoxybenzene-1,2-diamine, 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.

13.1 r3-(2-Amino-3-methoxy-phenylcarbamoyl)-propyll-methyl-carbamic acid benzyl esterTo a solution of 1.40 g 4-(benzyloxycarbonyl-methyl-amino)-butyric acid (obtained from 4- (methylamino)butyric acid and benzylchloroformate) in 25 mL THF were added 2.9 mL of DIPEA, 0.97 g of HOBt and 1.38 g EDC. After stirring for 5 min 0.80 g of 3-methoxy- benzene-1 ,2-diamine were added and the mixture was stirred for 3 h at rt. Sat. aq. NaHCOs solution was added, the phases were separated and the organic phase was washed with brine. The combined organic phases were dried over MgSO4, and concentrated in vacuo.LC-MS (A): tR = 0.80 min; [M+H]+: 372.27.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Methoxybenzene-1,2-diamine, and friends who are interested can also refer to it.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; HILPERT, Kurt; HUBLER, Francis; RENNEBERG, Dorte; WO2010/46855; (2010); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

These common heterocyclic compound, 1484-26-0, name is 3-Benzyloxyaniline, 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. SDS of cas: 1484-26-0

General Procedure: Aniline (10, 10 mmol), 2-chloroethanol (2 mL), CaCO3 (2.00 g, 20 mmol) and KI (10percent mmol) were added to 14 mL water and refluxed for 8 h. After filtration, the filtrate was extracted with EtOAc (14 mL.x.3), and the combined organic layers were washed with saturated NaCl (14 mL.x.2), dried over anhydrous Na2SO4, filtered and concentrated. Column chromatography afforded the desired product 11.

The synthetic route of 3-Benzyloxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lin, Song-Wen; Sun, Qi; Ge, Ze-Mei; Wang, Xin; Ye, Jia; Li, Run-Tao; Bioorganic and Medicinal Chemistry Letters; vol. 21; 3; (2011); p. 940 – 943;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 82172-73-4, name is O-(2-Methoxyethyl)hydroxylamine hydrochloride, 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 82172-73-4, Formula: C3H10ClNO2

General procedure: To a solution of bis(4-hydroxy)benzophenone (100 mg, 0.46 mmol) in EtOH (2 mL) was added hydroxylamine HCl (69 mg, 0.99 mmol) at ambient temperature. The reaction mixture was stirred until complete consumption of the starting material on TLC and quenched with H2O. The resulting mixture was diluted with EtOAc, and the organic phase was washed with H2O and brine, dried over MgSO4 and concentrated in vacuo Purification of the residue via flash column chromatography on silica gel (EtOAc : Hexane = 1 : 5 to 1 : 3) afforded 90 mg (84 %) of 12a as colorless liquid.

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, O-(2-Methoxyethyl)hydroxylamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kim, Taelim; Kim, Hye-In; An, Ji-Young; Lee, Jun; Lee, Na-Rae; Heo, Jinyuk; Kim, Ji-Eun; Yu, Jihyun; Lee, Yong Sup; Inn, Kyung-Soo; Kim, Nam-Jung; Bioorganic and Medicinal Chemistry Letters; vol. 26; 7; (2016); p. 1844 – 1848;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 171290-52-1, 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. 171290-52-1 name is 3,5-Dimethoxyphenylacetylene, 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.

General procedure: The azido derivative of N,-C terminal protected L-serine (1.0equiv) was taken in a 5:1 dry THF and water mixture solvent anddegassed it for 5 min with nitrogen gas. Then, terminal alkyne(1.1 equiv) was added with continuing stirring and degassing forthe next 5 min. Then 6 mol% sodium ascorbate and 1 mol% powderCuSO4 were added. The reaction mixture was degassed and allowed to proceed 18-20 h about 65-70 C. After total consumptionof the starting azide, the reaction mixture evaporatedcompletely and work up done by EtOAc and NH4Cl solution. Theorganic layer was washed with brine, dried over Na2SO4. Thesynthesized trizolyl amino acids were separated by column chromatography(si-gel, PE/EA = 1:1) and characterized. The averageyields were 50-85%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Dimethoxyphenylacetylene, and friends who are interested can also refer to it.

Reference:
Article; Bag, Subhendu Sekhar; Jana, Subhashis; Pradhan, Manoj Kumar; Bioorganic and Medicinal Chemistry; vol. 24; 16; (2016); p. 3579 – 3595;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 34967-24-3, name is 3,5-Dimethoxybenzyl 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 34967-24-3, Recommanded Product: 34967-24-3

To a stirred solution of 2,4 dichloro-pyrido [2,3-d] pyrimidine (1.3 g, 6.7 mmol) and 3, 5-dimethoxybenzylamine (1.1 g, 6.7 mmol) in 30 mL EtOH at RT was added TEA (4 mL, 28.7 mmol). A precipitate formed that was filtered off and washed with cold EtOH followed by hexanes to give 1.8 g of the title compound (82%) as a solid. mp 185C (dec).’H-NMR (DMSO-d6) 8 : 9.5 (t, 1H), 8. 9 (dd, 1H), 8.7 (dd, 1H), 7.5 (m, 1H), 6.5 (d, 2H), 6.4 (t, 1H), 4.6 (d, 2H), 3.7 (s, 6H). MS (m/z, %): 331 (100).

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.

Reference:
Patent; PFIZER PRODUCTS INC.; WO2005/61497; (2005); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 123652-95-9, name is (3-Fluoro-4-methoxyphenyl)methanamine, A new synthetic method of this compound is introduced below., Formula: C8H10FNO

General procedure: A microvawe vial (ovendried and under argon) was chargedwith the corresponding bromoindazole derivative (1.0 equiv.), theappropriate amine (1.2 equiv.), Pd(OAc)2 (5 mol%), BrettPhos(10 mol%), Cs2CO3 (1.5 equiv.) and anhydrous dioxane (0.2 mmol/mL). The vial was capped properly, flushed with argon and heatedto 120 C overnight. After cooling, the reaction mixture wasconcentrated under vacuum. The crude residue was diluted withwater and the aqueous phase was extracted 3 times with EtOAc.The organic layers were combined, washed with brine, dried overNa2SO4, filtered, concentrated and purified by silica gel columnchromatography, using the appropriate heptanes:EtOAc mixture.

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:
Article; Bollenbach, Maud; Lugnier, Claire; Kremer, Melanie; Salvat, Eric; Megat, Salim; Bihel, Frederic; Bourguignon, Jean-Jacques; Barrot, Michel; Schmitt, Martine; European Journal of Medicinal Chemistry; vol. 177; (2019); p. 269 – 290;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Synthetic Route of 89282-70-2, A common heterocyclic compound, 89282-70-2, name is 2-Methoxy-2-methylpropan-1-amine, molecular formula is C5H13NO, 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.

[0407] In Examples, a room temperature usually indicates10 to 30 C. ?H NMR indicates a proton nuclear magnetic resonance spectrum, and chemical shift (6) is expressed in ppm, using tetramethylsilane as an internal standard substance.; [0424] The intermediate compound (1) (0.24 g, 1.0 mmol), 2-methoxy-2-methylpropylamine (0.13 g, 1.2 mmol), and HOST (0.01 g, 0.1 mmol) were added to chloroform (Amylene-added product) (2.5 mE). Afier EDCD (0.24 g, 1.2 mmol) was added to the mixed liquid at room temperature, the mixture was stirred at room temperature for 3 hours. Thereafier, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with chloroform two times. After the organic layer was passed through a short column to remove impurities, this was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.24 g of a compound offollowing formula: (hereinafier, referred to as compound (8)).; [0425] ?H-NMR (CDC13, TMS, oe(ppm)): 1.21 (6H, s),3.23 (3H, s), 3.46 (2H, d), 4.61 (2H, s), 4.65 (2H, s), 6.73(1H, s), 7.10 (1H, br s), 7.30-7.40 (5H, m)

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:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; MITSUDERA, Hiromasa; OKAJIMA, Mayumi; KOWATA, Ayano; AWASAGUCHI, Kenichiro; UJIHARA, Kazuya; (108 pag.)US2017/295789; (2017); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 321-28-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 321-28-8, name is 1-Fluoro-2-methoxybenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Synthesis of 3-fluoro-4-methoxybromobenzene Into a flask of 5 l were charged 384 g (3.04 mol) of 2-fluoroanisole and 2.5 l of chloroform, to which was added dropwise 504 g (3.16 mol) of bromine over about 3 hours while cooling on an ice water bath at 10 C. The resulting mixture was stirred at room temperature over a night and heated under reflux for 8 hours. After the air cooling, the product was added with 1 l of water and 50 g of sodium bisulfite and sufficiently shaken to separate into two layers. The resulting organic layer was washed with an aqueous solution of 5% sodium hydrogen carbonate and further with 1 l of water and dried on magnesium sulfate. After magnesium sulfate was filtered off, the filtrate was concentrated and distilled under a reduced pressure (4 mmHg, bp: 93-96 C.) to obtain 585 g (yield: 94%) of 3-fluoro-4-methoxybromobenzene.

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, 1-Fluoro-2-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nippon Mining Co., Ltd.; US5098602; (1992); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem