Tag: M.W=100-200

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. 93919-56-3, name is (4-(Trifluoromethoxy)phenyl)methanamine, A new synthetic method of this compound is introduced below., Quality Control of (4-(Trifluoromethoxy)phenyl)methanamine

General procedure: To a solution of 2-(dibenzo[b,d]thiophen-2-yl)imidazo[1,2-a]pyridine-3-carboxylic acid 5 (2.83mmol) in anhydrous DMF (10mL) were added 1-[3-(dimethyl amino)propyl]-3-ethylcarbodiimide (EDCI, 3.84mmol), 1-hydroxybenzo triazole (HOBt, 1.54mmol), triethyl amine (TEA, 5.12mmol) and 6a-s (2.56mmol) at room temperature, and the resulting solution was heated at 80C with stirring. After 12h, the reaction mixture was cooled to room temperature and evaporated. Water (50mL) was added into the crude residue, the resulting solid was collected by filtration, and the filtered cake was washed with water (50mL) and dried to afford crude product. The resulting crude compound was purified by column chromatography over silica gel (n-hexane/EtOAc=1:1) to give 7a-s as a white solid.

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; Pulipati, Lokesh; Sridevi, Jonnalagadda Padma; Yogeeswari, Perumal; Sriram, Dharmarajan; Kantevari, Srinivas; Bioorganic and Medicinal Chemistry Letters; vol. 26; 13; (2016); p. 3135 – 3140;,
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Reference of 4179-19-5, 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. 4179-19-5, name is 3,5-Dimethoxytoluene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Stage 1 300 ml of a solution (1.6M) of butyllithium in hexane are added dropwise at room temperature to a solution of 73 g of 3,5-dimethoxytoluene in 450 ml of diethyl ether. The reaction mixture is heated at reflux for 3 hours under an inert atmosphere, the reaction mixture is then cooled to -60 C. and 99.7 g of methyl borate are added dropwise over 60 minutes. The reaction mixture is left at -60 C. for 3 hours and left to return to room temperature. The reaction mixture is stirred at room temperature for 16 hours, 6N hydrochloric acid is then added to the reaction mixture (pH=1) and the reaction mixture is left to separate by settling. The organic phase is recovered. The aqueous phase is extracted with diethyl ether. The combined organic phases are dried over anhydrous sodium sulphate. Evaporation of the solvent leaves a yellow oil which crystallizes by cooling to 0 C. After drying, white crystals of 2,6-dimethoxy-4-methylphenylboronic acid are recovered, M.p.=108 C., Yield 80%.

The synthetic route of 3,5-Dimethoxytoluene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sanofi; US5731340; (1998); A;,
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Related Products of 64465-53-8,Some common heterocyclic compound, 64465-53-8, name is 4-Fluoro-3-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.

4-Fluoro-3-methoxyphenylhydrazine Hydrochloride To stirred hydrochloric acid (100 mL) at 0 C. was added 3-methoxy-4-fluoroaniline (10 g, 71 mmol) followed by water (10 mL) and more hydrochloric acid (10 mL). The mixture was warmed to room temperature, stirred for 20 min then cooled to -5 C. A solution of sodium nitrite (5.14 g, 75 mmol) in water (25 mL) was added dropwise such that the internal temperature remained below 0 C. The mixture was warmed to room temperature and stirred for 2 h. The mixture was cooled to -5 C. and a solution of tin(II)chloride dihydrate (64 g, 284 mmol) in hydrochloric acid (200 mL) was added dropwise such that the internal temperature remained below 0 C. The mixture was warmed to room temperature, stirred for 3 h then filtered. The filter-cake was washed with hydrochloric acid and dried in vacuo to give a pink solid (7.4 g). The emerging precipitate from the combined filtrates was filtered-off, washing with hydrochloric acid, to give a further crop of product (1.8 g. Combined yield 9.2 g, 67%); m.p. 250+ C. (dec.); NMR: (400 MHz, DMSO-d6) deltaH10.17 (3H, s, NH3), 8.14 (1H, s, NH), 7.15 (1H, dd,J 11.6, 8.6 Hz), 6.95 (1H, dd, J 7.6, 3.0 Hz), 6.54 (1H, dt, J 8.6, 3.0 Hz), 3.83 (3H, s, MeO).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Fluoro-3-methoxyaniline, its application will become more common.

Reference:
Patent; Bentley, Jonathan Mark; Davidson, James Edward Paul; Mansell, Howard Langham; Monck, Nathaniel Julius Thomas; US6479534; (2002); B1;,
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Related Products of 89282-70-2, 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. 89282-70-2, name is 2-Methoxy-2-methylpropan-1-amine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 3 Synthesis of N-(2-methoxy-2-methylpropyl) formamide Formic acid (19.2 g, 0.40 mol) and acetic anhydride (40.8 g, 0.40 mol) Were combined and heated to 45-50 C. for one hour and cooled to approximately 0 C. in an ice/acetone bath. A solution of 2-methoxy-2-methylpropyl-1-amine (36 g, 0.35 mol), precooled to approximately 0 C. in an ice/acetone bath was added slowly while keeping the temperature of the mixture below 12 C. After the addition was complete, the mixture was allowed to warm slowly to room temperature and was stirred at room temperature overnight. The solution was evaporated and the residue distilled at 97-107 C./1-2 mm Hg. to give 43.2 g (94%). NMR (CDCl3): delta 1.2 (s, 6H, CH3), 3.3 (m, 5H, CH3 O and CH2), 6.6 (b, 1H, NH), 8.2 (bs, 1H, HCO).

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-Methoxy-2-methylpropan-1-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. Du Pont de Nemours and Company; US4988827; (1991); A;,
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Synthetic Route of 6851-80-5, These common heterocyclic compound, 6851-80-5, name is 1-(2-Methoxyphenyl)-N-methylmethanamine, 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.

General procedure: To a suspension of the corresponding secondary amine (3.22 mmol) and anhydrous K2CO3 (765 mg, 5.48 mmol) in CH3CN (20 mL) was added the intermediates 3-5 (0.60 mmol). The mixture was refluxed for 6-8 h. The solvent was removed under reduced pressure. The residue was diluted with water (30 mL) and the mixture was extracted with dichloromethane (30 mL×3). The combined organic phases were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified on a silica gel chromatography in petroleum ether/acetone (20/1, v/v) to afford compound 7-9

Statistics shows that 1-(2-Methoxyphenyl)-N-methylmethanamine is playing an increasingly important role. we look forward to future research findings about 6851-80-5.

Reference:
Article; Song, Qing; Li, Yan; Cao, Zhongcheng; Qiang, Xiaoming; Tan, Zhenghuai; Deng, Yong; Bioorganic Chemistry; vol. 84; (2019); p. 137 – 149;,
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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. 171290-52-1, name is 3,5-Dimethoxyphenylacetylene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3,5-Dimethoxyphenylacetylene

General procedure: Azide 13 (300 mumol), alkyne (750 mumol), CuSO4 (9.6 mg, 60 mumol) and sodium ascorbate (60.0 mg, 300 mumol) were dissolved in 1:1 t-BuOH/H2O (3 mL). The mixture was stirred for 2 h at rt. After the completion of the reaction, the mixture was filtered and washed with H2O (70 mL) (solid A). The filtrate was extracted with EtOAc (3 * 70 mL). The combined organic extracts were dried over anhyd MgSO4, filtered, and concentrated by rotary evaporation (residue B). The solid A and residue B were combined and purified by column chromatography to afford 8 or 9.

According to the analysis of related databases, 171290-52-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Song, Doohee; Park, Yunjeong; Yoon, Jieun; Aman, Waqar; Hah, Jung-Mi; Ryu, Jae-Sang; Bioorganic and Medicinal Chemistry; vol. 22; 17; (2014); p. 4855 – 4866;,
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Application of 41789-95-1, A common heterocyclic compound, 41789-95-1, name is 1-(3-Methoxyphenyl)-N-methylmethanamine, 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.

Step B: To a solution of the above amine (6.2 g, 41.00 mmol) from Step A in methylene chloride (100 mL) was added 3,4-dichlorophenacyl bromide (10.0 g, 37.3 mmol) and the resulting mixture was stirred at 0 0C for 1 hour prior to the addition of triethylamine (5.20 mL, 37.31 mmol), followed by 1 hour stirring at 0 0C. The reaction mixture was diluted with water (100 mL) then the aqueous phase was extracted with additional methylene chloride (3 x 75 mL). The combined extracts were dried over sodium sulfate, filtered, and concentrated to afford l-(3,4-dichlorophenyl)-2-((3- methoxybenzyl)(methyl)amino)ethanone (15.08 g) as a light yellow oil, which was used in the next step without further purification: 1H NMR (500 MHz, CDCl3) delta 8.08 (d, J = 2.0 Hz, IH), 7.78 (dd, J = 8.5; 2.0 Hz, IH), 7.50 (d, J = 8.5 Hz, IH), 7.25 (d, J= 8.5 Hz, IH), 6.90 (d, J= 7.5 Hz, IH), 6.87 (d, J= 2.5 Hz, IH), 6.82 (dd, J= 8.0; 2.5 Hz, IH), 3.79 (s, 3H), 3.66 (s, 2H), 3.60 (s, 2H), 2.33 (s, 3H).

The synthetic route of 41789-95-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALBANY MOLECULAR RESERCH, INC.; WO2010/132442; (2010); A1;,
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Synthetic Route of 592-55-2, These common heterocyclic compound, 592-55-2, name is 1-Bromo-2-ethoxyethane, 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.

To a 250 mL flask, 2-bromoethyl ether (37.62 g, 0.246 mol),4-hydroxybenzaldehyde (32 g, 0.262 mol), anhydrous potassiumcarbonate (67.89 g, 0.491 mol) and 120 mL acetonitrilewere added. The solution was heated to reflux for 24 h.Then, the solvent was evaporated in vacuo and the residuewas dissolved in H2Oand extracted with ethyl acetate. Theorganic layers were washed with 2× 100 mL sodium hydroxidesolution (1 N) and with 2× 100 mL saturated brine,respectively. The obtained solution was concentrated to getthe pure product, yield 81%. 1H NMR (400 MHz, CDCl3)delta 9.72 (s, 1H, CHO), 7.68 (m, 2H, benzyl), 6.89 (m, 2H,benzyl), 4.05 (t, 2H, OCH2CH2O), 3.67 (t, 2H, OCH2CH2O),3.45 (q, 2H, -CH2CH3), 1.09 (t, 3H, CH3). Mass (ESI): calcdfor C11H14O3(M + H)+, 195.27; found 195.52.

Statistics shows that 1-Bromo-2-ethoxyethane is playing an increasingly important role. we look forward to future research findings about 592-55-2.

Reference:
Article; Wu, Fengshou; Yang, Mengqian; Zhang, Juan; Zhu, Sizhe; Shi, Mengge; Wang, Kai; Journal of Biological Inorganic Chemistry; vol. 24; 1; (2019); p. 53 – 60;,
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Electric Literature of 115144-40-6, These common heterocyclic compound, 115144-40-6, name is 3,4-Difluoroanisole, 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.

a) 7.29 ml (66.3 mmol) of titanium tetrachloride were added while stirring to a solution, cooled to 0, of 5.73 g (39.8 mmol) of 3,4-difluoroanisole in 30 ml of anhydrous dichloromethane. Subsequently, the mixture was treated dropwise over 10 minutes with 3.51 ml (39.6 mmol) of 1,1-dichloromethyl methyl ketone and stirred at room temperature for one hour. The mixture was poured into 100 ml of ice-water, extracted twice with 150 ml of dichloromethane each time and the combined organic phases were washed once with 100 ml of water and once with 100 ml of saturated sodium chloride solution. After drying over magnesium sulphate concentration was carried out in a vacuum. The crude product obtained was purified by column chromatography on silica gel (hexane/ethyl acetate 4:1). There were obtained 5.8 g (84%) of 4,5-difluoro-2-methoxybenzaldehyde as a white solid with m.p. 74.

Statistics shows that 3,4-Difluoroanisole is playing an increasingly important role. we look forward to future research findings about 115144-40-6.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; EP906301; (2002); B1;,
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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. 64465-53-8, name is 4-Fluoro-3-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H8FNO

Description 34; 5-[(4-Fluoro-3-methoxvphenvl) aminolmethvlene}-2, 2-dimethvl- 1 3-dioxane-4, 6-dione; To a stirred solution of 4-fluoro-3-methoxyaniline (20 g, 142 mmol) in acetonitrile (200 ml) was added 2, 2-dimethyl-1, 3-dioxane-4,6-dione (Meldrum’s acid) (22.5 g, 156 mmol) followed by trimethyl orthoformate (18.6 ml, 170 mmol). The mixture was heated to reflux for 3 hours. The cooled mixture was filtered to give the title compound (30.9 g, 74%). 1H NMR (400 MHz, CDCl3) 1.76 (6 H, s), 3.94 (3 H, s), 6.76-6. 83 (2 H, m), 7.14 (1 H, dd, J10. 5 and 8.4), 8.56 (1 H, d, J14. 4), 11.23 (1 H, d, J14.4).

According to the analysis of related databases, 64465-53-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK SHARP & DOHME LIMITED; WO2005/47279; (2005); A1;,
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