Amides-buliding-blocks

These common heterocyclic compound, 104863-65-2, name is N-Methoxy-N-methylpropionamide, 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: 104863-65-2

Cool a solution of 1-bromo-2-methyl-4-(trifluoromethyl)benzene (2.00 g, 8.367 mmol) and THF (17 mL) to -71 C., and then add n-butyl lithium (2.5 M in hexanes, 9.204 mmol, 3.681 mL) over 5 minutes. Stir the mixture for 15 minutes at -71 C. Add N-methoxy-N-methylpropanamide (0.980 g, 8.367 mmol) to the mixture drop-wise over 3-4 minutes keeping temperature below -65 C. Continue to stir the solution at -71 C. for 15-20 minutes; then warm the solution to room temperature. Stir at room temperature for 40 minutes. Quench the reaction with a saturated ammonium chloride aqueous solution. Extract the aqueous layer with Et2O. Wash the combined organic extracts with water and brine. Dry the mixture over sodium sulfate; filter; collect the filtrate; and concentrate the filtrate under reduced pressure. Purify the residue by flash chromatography (40 g RediSep column) eluting with a gradient of 0-40% DCM/pentane to give the title compound as a colorless oil (1.490 g, 82% yield). 1H NMR (399.80 MHz, d6-DMSO) delta 7.84 (d, J=7.8 Hz, 1H), 7.64-7.61 (m, 2H), 2.93 (q, J=7.1 Hz, 2H), 2.39 (s, 3H), 1.03 (t, J=7.2 Hz, 3H).

The synthetic route of N-Methoxy-N-methylpropionamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; US2012/302608; (2012); A1;,
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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. 177906-48-8, name is trans-N-Boc-1,4-cyclohexanediamine belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of trans-N-Boc-1,4-cyclohexanediamine

tert-Butyl (lr,4r)-4-(dimethylamino)cyclohex lcarbamate (SB1-E-21-2) To a solution of SB1-E-21-1 (850 mg, 3.97 mmol) and HCHO (600 mg, 20.0 mmol) in MeOH (30 mL) was added NaBH3CN (1.1 g, 17.5 mmol), the mixture was stirred at r.t overnight, after completion, concentrated to remove the solvent, the residue was extracted with ethyl acetate (100 mL chi 4), the organic phase was washed with brine (50 mL chi 2), dried with Na2S04. Filtered, concentrated to remove the solvent, the residue was purified by silica gel (DCM/MeOH = 10/1, 5/1) to obtain SB1-E-21-2 (light brown solid, 800 mg, yield 83%). LCMS (m/z): 243 [M + H]+.

The synthetic route of 177906-48-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DANA-FARBER CANCER INSTITUTE, INC.; GRAY, Nathanael, S.; ZHANG, Tinghu; KWIATKOWSKI, Nicholas, Paul; (299 pag.)WO2016/160617; (2016); A2;,
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Electric Literature of 5349-24-6, 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. 5349-24-6, name is N-Butyl-2-chloroacetamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Various substituted anilines were dissolved in glacial acetic acid at0 C, to this was added over 30 min choloroacetyl chloride (2 equivalents).The reaction mixture was brought to room temperature andstirred overnight. Saturated sodium bicarbonate solution was added tillcomplete neutralization. The resulting precipitate was filtered off andwashed with n-hexane and dried. The resultant product (1) was usedfurther without any purification. Either of 4-hydroxy benzaldehyde(2a), vanillin (2b) or isovanillin (2c) (1 equivalent) was dissolved inacetone and potassium carbonate (2 equivalents) was added. Thencorresponding substituted acetamide (1) was mixed to the stirring solution.Finally, potassium iodide (1.5 equivalent) was added. The reactionmixture was refluxed for 8-10 h. After completion of reaction,the resultant mixture was concentrated and treated with water andextracted with ethyl acetate (3×20 mL). The organic layers werecombined and treated with brine and dried over sodium sulfate andconcentrated. The crude mixture was purified over silica gel (60-120)using petroleum ether: ethyl acetate (9:1).

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, N-Butyl-2-chloroacetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Sonawane, Vinay R.; Siddique, Mohd Usman Mohd; Gatchie, Linda; Williams, Ibidapo S.; Bharate, Sandip B.; Jayaprakash, Venkatesan; Sinha, Barij N.; Chaudhuri, Bhabatosh; European Journal of Pharmaceutical Sciences; vol. 131; (2019); p. 177 – 194;,
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Reference of 6274-22-2,Some common heterocyclic compound, 6274-22-2, name is 4-Amino-N-methylbenzamide, molecular formula is C8H10N2O, 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: CS2 (50 mL) was added to a stirring mixture of DABCO (30 mmol) and amine (10 mmol) in acetone (10 mL). The resulting mixture was further stirred at room temperature to achieve dithiocarbamate, and the process of the reaction was monitored by TLC. After completion of the reaction, the solution was filtered and the solid was washed with acetone. After it was dried in an infrared-ray oven, the salt was dissolved in dried CHCl3 (10 mL) and the mixture was chilled to 0-5 C in an ice bath. BTC (1010 mg, 3.4 mmol), dissolved in CHCl3 (5 mL), was added dropwise for 30 min with constant stirring. The reaction mixture was then allowed to reach room temperature and stirred for a further 4 h. Triethylenediammmonium hydrochloride was filtered off, and the filtrate was evaporated in vacuo to afford the desired isothiocyanate in good purity. All products were identified by comparison with authentic samples.

The synthetic route of 6274-22-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Pengfei; Li, Chunyan; Zhang, Jingwei; Xu, Xiaoyong; Synthetic Communications; vol. 43; 24; (2013); p. 3342 – 3351;,
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Adding a certain compound to certain chemical reactions, such as: 5900-59-4, name is 2-Amino-4-chlorobenzamide, belongs to amides-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 5900-59-4, Safety of 2-Amino-4-chlorobenzamide

[00394] Step B: To a solution of 2-amino-4-chlorobenzamide (393 mg, 2.30 mmol) and DIEA (0.60 mL, 3.45 mmol) in THF (15 mL) at 0 0C was added ethyl chlorooxoacetate (0.28 mL, 2.53 mmol). The solution was allowed to warm to rt and stir for 2 h. The mixture was concentrated under reduced pressure and the residue was purified by silica gel chromatography eluting with 10-50percent EtOAc/hexanes to afford ethyl 2-(2-carbamoyl-5-chlorophenylamino)-2-oxoacetate as a solid (545 mg, 88percent). 1H NMR (300 MHz, DMSO-d6) delta 1.32 (t, J= 6.97 Hz, 3 H), 4.31 (q, J= 6.97 Hz, 2 H), 7.34 (d, J= 8.48 Hz, 1 H), 7.86 – 8.03 (m, 2 H), 8.44 (br s, 1 H), 8.62 (s, 1 H), 13.24 (s, 1 H)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Amino-4-chlorobenzamide, and friends who are interested can also refer to it.

Reference:
Patent; AMBIT BIOSCIENCES CORPORATION; LIU, Gang; CHAO, Qi; HADD, Michael, J.; HOLLADAY, Mark, W.; ABRAHAM, Sunny; SETTI, Eduardo; WO2010/99379; (2010); A1;,
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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. 7150-72-3, name is tert-Butyl vinylcarbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of tert-Butyl vinylcarbamate

General procedure: A 10 mL round-bottomed flask equipped with a rubber septum and a magnetic stir bar was charged with 1 (1.0 equiv), 2 (2.5 equiv), 3 (2.0 equiv), and fac-Ir(ppy)3 (0.01 equiv). The flask was evacuated and backfilled 3 times with N2. DMSO was then added with syringe under N2. The mixture was then irradiated by white LED strips. After completion of the reaction (6 h, as judged by TLC analysis), the mixture was poured into a separatory funnel containing sat. aq NaHCO3 (20mL) and EtOAc (20 mL). After extraction with EtOAc, the organic layer was separated, dried (Na2SO4), and concentrated under reduced pressure after filtration. The crude product was purified by flash chromatography on silica gel to afford the desired product 4.

The synthetic route of 7150-72-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; An, Xiao-De; Yu, Shouyun; Synthesis; vol. 50; 17; (2018); p. 3387 – 3394;,
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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. 138-41-0, name is Carzenide, A new synthetic method of this compound is introduced below., Safety of Carzenide

General procedure: To a stirred solution of the carboxylic acid (1.0 mmol) in anhydrous CH2Cl2 (5 mL), the appropriate amine or its hydrochloric acid(1 mmol), Et3N (1 eq, 0.14 mL, 1 mmol or 2 eq, 0.28 mL, 2 mmol in caseof hydrochloric acid), HOBt (1 eq, 140 mg, 1 mmol) and EDCI (1.1 eq,211 mg, 1.1 mmol) were added at 0 C. The reaction mixture was stirred overnight at room temperature and then the solvent was removedunder reduced pressure. The residue was dissolved in AcOEt and washedwith H2O, 5% H2SO4, H2O, 5% NaHCO3, brine and H2O. In thecase of proline washing with 5% H2SO4, was omitted. The product was obtained after drying the organic phase over anhydrous Na2SO4, evaporation of the solvent under reduced pressure, and purification by column chromatography.

The synthetic route of 138-41-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Afantitis, Antreas; Aidinis, Vassilis; Gerokonstantis, Dimitrios Triantafyllos; Kokotos, George; Magkrioti, Christiana; Moutevelis-Minakakis, Panagiota; Nikolaou, Aikaterini; Bioorganic and medicinal chemistry; vol. 28; 2; (2020);,
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Adding a certain compound to certain chemical reactions, such as: 42137-88-2, name is N,N-Bis(2-chloroethyl)-4-methylbenzenesulfonamide, belongs to amides-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 42137-88-2, Recommanded Product: N,N-Bis(2-chloroethyl)-4-methylbenzenesulfonamide

Alternatively, Intermediate 1 can be prepared from commercially available starting materials 5-iodo-methoxyaniline and N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide. Treatment of 5-iodo-methoxyaniline and N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide with sodium carbonate and potassium iodide in cyclohexanol at 160 C. will provide 1-(5-iodo-2-methoxyphenyl)-4-tosylpiperazine. Coupling of 1-(5-iodo-2-methoxyphenyl)-4-tosylpiperazine with sodium 3-(difluoromethoxy)benzenesulfinate can be accomplished by treatment with Xantphos, cesium carbonate, and tetrabutyl ammonium chloride. The resulting 1-(5-(3-(difluoromethoxy)phenylsulfonyl)-2-methoxyphenyl)-4-tosylpiperazine can be converted to Intermediate 1 by treatment with concentrated sulfuric acid at 50 C. for 5 hours.

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, N,N-Bis(2-chloroethyl)-4-methylbenzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Black, Lawrence A.; US2014/120036; (2014); A1;,
Amide – Wikipedia,
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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. 147356-78-3, name is N-Methoxy-N-methylcyclopropanecarboxamide, A new synthetic method of this compound is introduced below., Formula: C6H11NO2

To the reaction flask, 2-(2-methoxyphenoxy)tetrahydropyran (8B) (200 g, 0.96 mol) and tetrahydrofuran (1000 ml) were added under nitrogenatmosphere, cooled to -20 C. with dry ice acetonebath, added nButyllithium(460 mL, 1.15 mol, 2.5M, Energy Chemical) dropwise slowly,stirred at -10 C. for 2 h. N-methyl-N-methoxyacetamide(186 g, 1.44 mol) was added and stirred at room temperature overnight. The reactionmixture was quenched with a saturated ammonium chloride solution (1000 mL), the organic phase was collected, washed with water (1000mL×2), brine (1000 mL×2), dried over anhydrous sodium sulfate and concentrated under vacuum to obtain cyclopropyl-(3-methoxy-2-tetrahydropyran-2-yloxy-phenyl)methanone (8C) as a red liquid (280 g, crude product), which was submitted to the next step without furtherpurification

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; Sichuan Haisco Pharmaceutical Co., Ltd; Chin, Rinrin; Li, Fang chiong; Lee, Swi Swi; Luo, Huadong; Luo, Sin Pong; Wan, songrin; Ron, Ray; Liu, Guoliang; Wei, Yonggang; Liu, Chien Wi; Tang, Peongcho; (148 pag.)KR2016/5361; (2016); A;,
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Related Products of 63920-73-0, A common heterocyclic compound, 63920-73-0, name is 2-Amino-4,6-dimethoxybenzamide, molecular formula is C9H12N2O3, 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.

Example 20. Preparation of 2-[4-(2-hydroxy-ethoxy)-phenyl]-5,7-dimethoxy-3H-quinazolin-4-one [0239] To a flask (250 mL) with a magnetic stirrer were added 4-hydroxybenzalde (10.0 g, 81.8 mmol), 2-chloroethanol (26.3 g, 327 mmol), potassium carbonate (22.6 g, 163 mmol), and ethanol (80 mL). The reaction mixture was stirred at 700C for 16 hours. Potassium carbonate was filtered and ethanol was removed. The residue was diluted with ethyl acetate (200 ml_) and washed with 5% sodium hydroxide (100 ml_), water (100 ml_), and brine (100 ml_). The crude product was purified by column chromatography (silica gel, 230-400 mesh), using hexane / ethyl acetate (1 :1) as eluent, to afford 4-(2-hydroxy-ethoxy)-benzaldehyde. Yield: 10.0 g (73%).[0240] To a solution of 2-amino-4,6-dimethoxy-benzamide (0.400 g, 2.00 mmol) and 4-(2-hydroxy-ethoxy)-benzaldehyde (0.340 g, 2.00 mmol) in N, N- dimethylacetamide (8 ml_) were added NaHSO3 (0.390 g, 2.20 mmol) and p-TSA (38 mg, 0.20 mmol). The reaction mixture was stirred at 115-1200C for 5 hours and cooled to room temperature. The solvent was removed under reduced pressure. The residue was diluted with water (40 ml_) and the solid was collected, mixed with methanol (50 ml_), and stirred for 30 min. The solid was filtered and rinsed with ether (30 ml_) to give the title compound as white solid. Yield: 0.42 g (61%). 1H NMR (400 Hz, DMSO-d6): delta 11.98 (s, 1H), 8.18 (d, 2H), 7.08 (d, 2H), 6.78 (s, 1 H), 6.52 (s, 1H), 4.98 (s, 1 H), 4.10 (t, 2H), 3.90 (s, 3H), 3.84 (s, 3H)1 3.74 (t, 2H). MS (ES+) m/z: 343.13 (M+1).

The synthetic route of 63920-73-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RESVERLOGIX CORP.; HANSEN, Henrik, C.; WAGNER, Gregory, S.; ATTWELL, Sarah, C.; MCLURE, Kevin, G.; KULIKOWSKI, Ewelina, B.; WO2010/123975; (2010); A1;,
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