Amides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 1943-79-9, name is Phenyl methylcarbamate, 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 1943-79-9, Recommanded Product: 1943-79-9

Production Example 19-7 5-((2-Aminopyridin-4-yl)oxy)-6-(difluoromethoxy)-N-methyl-1H-indole-1-carboxamide 4-((6-(Difluoromethoxy)-1H-indol-5-yl)oxy)pyridin-2-amine described in Production Example 19-6 (4.4 mg, 0.015 mmol) was dissolved in N,N-dimethylformamide (500 muL), then 50-72% oily sodium hydride (4.1 mg) was added under nitrogen atmosphere at 0 C., and the mixture was stirred at room temperature for 30 minutes. The mixture was cooled to 0 C. again and phenyl methylcarbamate described in Production Example 1-7 (16.4 mg, 0.108 mmol) was added, and the mixture was stirred at room temperature for 50 minutes. Water and ethyl acetate were added to the reaction mixture for partition. The organic layer was washed with a saturated saline solution, then dried over anhydrous sodium sulfate and filtered, and then the filtrate was concentrated under vacuum. The residue was dissolved in dichloromethane and the resultant was purified with NH silica gel column chromatography (n-heptane:ethyl acetate=1:1-0:1-ethyl acetate_methanol=99:1-9:1), and then the target fraction was concentrated under vacuum to obtain the title compound (4.3 mg, 82%). 1H-NMR Spectrum (CDCl3) delta (ppm): 3.08 (3H, d, J=4.8 Hz), 4.44 (2H, brs), 5.49 (1H, brs), 5.91 (1H, d, J=1.8 Hz), 6.26 (1H, dd, J=6.2, 2.2 Hz), 6.50 (1H, t, J=74.0 Hz), 6.61 (1H, d, J=3.7 Hz), 7.35 (1H, s), 7.41 (1H, d, J=3.7 Hz), 7.92 (1H, d, J=5.9 Hz), 8.23 (1H, s).

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Reference:
Patent; Eisai R&D Management Co., Ltd.; Funasaka, Setsuo; Okada, Toshimi; Tanaka, Keigo; Nagao, Satoshi; Ohashi, Isao; Yamane, Yoshinobu; Nakatani, Yusuke; Karoji, Yuki; US2014/235614; (2014); A1;,
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Adding a certain compound to certain chemical reactions, such as: 6325-93-5, name is 4-Nitrobenzenesulfonamide, 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 6325-93-5, HPLC of Formula: C6H6N2O4S

General procedure: A mixture of nitroarene (1 mmol), PdCu/graphene (6 mg) and sodium borohydride (2 mmol) were taken in a 25 mL reaction tube. 3 mL of EtOH:H2O (1:2 in volume ratio) was added by a syringe at 0 C. After 10 min the reaction mixture was placed in an oil bath at 50 C. The reaction was monitored by TLC. On completion, the reaction mixture was extracted with ethylacetate and dried ove ranhydrous Mg2SO4. Evaporation of the combined organic layer andfollowed by column chromatography over silica gel (60-120 mesh) afforded desired corresponding amines.

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Reference:
Article; Feng, Yi-Si; Ma, Jing-Jing; Kang, Yu-Mei; Xu, Hua-Jian; Tetrahedron; 36; (2014); p. 6100 – 6105;,
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Adding a certain compound to certain chemical reactions, such as: 180079-94-1, name is tert-Butyl 3-aminophenethylcarbamate, 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 180079-94-1, Formula: C13H20N2O2

Production Example 30 Production of 3′,4′-dihydro-2’H-spiro[cyclobutane-1,1′-isoquinolin]-6′-amine 2 mL of 85 % phosphoric acid was added to 350 mg of the compound obtained in Production Example 29-2), and stirred at 70C for 1 hour. Further, 0.144 mL of cyclobutanone was added to it, and reacted at 140C for 3 hours, using a microwave reactor. The reaction liquid was diluted with water, then potassium carbonate was added to it, and extracted with ethyl acetate. This was washed with saturated saline water, dried with anhydrous magnesium sulfate, and the solvent was evaporated away. The crude product was purified through basic silica gel column chromatography (hexane/ethyl acetate) to obtain 157 mg of the entitled compound as a colorless oily compound. 1H-NMR (CDCl3) delta: 7.28 (1H, d, J=8.3 Hz), 6.59 (1H, dd, J=8.3, 2.9 Hz), 6.37 (1H, d, J=2.4 Hz), 3.54 (2H, s), 3.03 (2H, t, J=5.9 Hz), 2.68 (2H, t, J=6.1 Hz), 2.47-2.40 (2H, m), 2.18-2.07 (3H, m), 2.02-1.92 (1H, m)

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, tert-Butyl 3-aminophenethylcarbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Banyu Pharmaceutical Co., Ltd.; EP2168966; (2010); A1;,
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Electric Literature of 4943-86-6, 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. 4943-86-6, name is 2-Amino-N-(4-chlorophenyl)benzamide, This compound has unique chemical properties. The synthetic route is as follows.

The reaction flask was added 1l (2mmol, 493mg),and then added tert-butyl nitrite (6mmol, 0.72mL),followed by tetrabutylammonium iodide (5mol%,37 mg of) and acetonitrile (20mL). Then the system was heated for 12 hours at 60 deg C. for air, vacuum spin dry acetateAfter the nitrile with petroleum ether / ethyl acetate = 6/1 mixed solvent of a simple column chromatography to give the product 2L, 86% yield. yellowsolid,

The chemical industry reduces the impact on the environment during synthesis 2-Amino-N-(4-chlorophenyl)benzamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Zhengzhou Institute of Light Industry; Yan, Yi zhe; Shi, Miao miao; Liu, Yan qi; Zhi, Huan huan; He, Yuan; Niu, Bin; (18 pag.)CN105418525; (2016); A;,
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Electric Literature of 142-78-9, 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. 142-78-9, name is N-(2-Hydroxyethyl)dodecanamide, This compound has unique chemical properties. The synthetic route is as follows.

33 mg (4.5 mol %) of KBr (co-catalyst) was dissolved in 6 mL of water. Tetrahydrofuran solvent THF (31 mL), AA-TEMPO catalyst (25 mg, 2.5 mol %) and 1.5 g N-lauroylethanolamide (LMEA) were added with stirring to give a homogeneous water-white solution. Sodium hypochloride oxidizing agent (22 mL of 11.5% aq. Solution, 6.5 equivalents) and 2.3 mL of 2 NaOH (to maintain pH above 7) were mixed. The combined solution was added dropwise to the solution of LMEA and catalyst over a period of 1.5 hour. A separate aqueous layer immediately formed upon addition of the sodium hypochlorite solution. The pH of the aqueous layer was 12.7 after addition of the first 3.5 ml. The temperature was maintained below 32 C. with an ice-water bath. The reaction was stirred for 0.5 hr. more until complete conversion of LMEA to LG as determined by reversed-phase High Pressure Liquid Chromatography, abbreviated HPLC. The pH at end of the reaction was 7.6.At completion of the reaction, the mixture was acidified to pH 3.0 (to get the purified carboxylic acid) by addition of 8.5 mL of 1 N HCl, and the layers were separated. The lower aqueous layer was extracted with 30 mL THF, and the combined THF layers were concentrated on a rotary evaporator and dried in vacuo to give N-lauroylglycine in 116% yield (residual water present); Example 2 Oxidation of LMEA with 3.25 eq. of NaOCl, and Acid Work-UpThe procedure in Example 1 was followed, except that the amount of sodium hypochlorite was decreased to 3.25 equivalents. The isolated yield was 103% (includes residual water), showing that the oxidation works with the lower sodium hypochlorite amount; Example 4Oxidation of LMEA in THF with 6.5 eq. of NaOCl, Drowning Procedure at pH=2.6The procedure of Example 1 was followed except for the isolation step. After completion of the reaction, the mixture was acidified to pH=2.6 with 9.25 mL of 1 N HCl. The entire reaction mixture (both THF and water phases) were poured in 240 mL of water with vigorous stirring. The precipitated product was isolated by gravity filtration, and washed with 200 mL water. After air-drying, and further drying in vacuo, the product was obtained in 77% yield. The yield can be improved by better filtration techniques, e.g. by pressure filtration through a 0.45 mum or less filter; Example 5Oxidation of LMEA in THF with 3.25 eq. of NaOCl, Drowning Procedure, Effect of pH on YieldThe procedure of Example 2 was followed except for the isolation step. After completion of the reaction, the mixture was only partially acidified (to pH=5.2 with 3.6 mL of 1 N HCl.) The entire reaction mixture (both THF and water phases) were poured in 240 mL of water with vigorous stirring. The precipitated product was isolated by gravity filtration, and washed with 240 mL water. After drying in vacuo overnight, the product was obtained in 59% yield (based on free carboxylic acid), and 55% (based on the sodium carboxylate). The lower yield than Example 4 is attributed to the larger proportion of the water-soluble sodium carboxylate at the higher pH.

The chemical industry reduces the impact on the environment during synthesis N-(2-Hydroxyethyl)dodecanamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Conopco, Inc.; US7307187; (2007); B1;,
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Synthetic Route of 75175-77-8,Some common heterocyclic compound, 75175-77-8, name is 3-(4-Fluorophenyl)-N,N-dimethylacrylamide, molecular formula is C11H12FNO, 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: General procedure: A mixture of appropriately substituted arylmethyl ketone (4 mmol) and DMF-DMA (20 mmol)was refluxed for8-12 h and monitored by TLC. After complete consumption ofsubstituted methyl ketone, the mixture was subjected to rotaryevaporation under reduced pressure to remove the excess of DMFDMAand the liberated methanol. After that DMSO (6-8 mL) and 4-azidobenzenesulfonamide (4 mmol) were added to reactionmixture. After addition, reaction mixture was allowed to stir at 90C for 8-10 h in silicon oil bath. After completion, reaction mixturewas poured into water to afford required product (7a-7j). Crudeproduct thus obtained was recrystalized with ethanol.

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

Reference:
Article; Kumar, Rajiv; Vats, Lalit; Bua, Silvia; Supuran, Claudiu T.; Sharma, Pawan K.; European Journal of Medicinal Chemistry; vol. 155; (2018); p. 545 – 551;,
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Adding a certain compound to certain chemical reactions, such as: 115643-59-9, name is 2-Amino-6-fluorobenzamide, 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 115643-59-9, Safety of 2-Amino-6-fluorobenzamide

An aromatic amine 1t-1 (0.20 mmol), a platensimycin acid (0.10 mmol), and2-(7-Azobenzotriazole)-N,N,N’,N’-tetramethyluronium hexafluorophosphate (HATU) (0.30 mmol) was added to the reaction flask and 1.0 ml was added.N,N-dimethylformamide, stirring at room temperature; slowly adding triethylamine (0.45 mmol), stirring for 12 hours, rotary evaporationSolvent to obtain a crude product, which is subjected to column chromatography to obtain a platensimycin analog2t-1, yield 42%.

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Reference:
Patent; Changsha Tianci Bio-pharmaceutical Technology Co., Ltd.; Changsha Cihang Pharmaceutical Institute Co., Ltd.; Ha Yao Cihang Pharmaceutical Co., Ltd.; Duan Yanwen; Shen Ben; Huang Yong; Zhu Xiangcheng; Qiu Lin; Tian Kai; (39 pag.)CN107793388; (2018); A;,
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Some common heterocyclic compound, 67442-07-3, name is 2-Chloro-N-methoxy-N-methylacetamide, molecular formula is C4H8ClNO2, 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. Recommanded Product: 67442-07-3

Example 10l-(4-teri-butoxy-2-isopropoxy-l,3-benzothiazol-7- l)-2-chloro-ethanoneA solution of n-butyllithium in hexanes (1.6 M, 0.41 mL, 0.65 mmoles) was added dropwise to a pre-cooled (-50 ¡ãC) solution of 7-bromo-4-tert-butoxy-2-isopropoxy-l,3-benzothiazole XVII (225 mg, 0.59 mmoles) in methyl tert-butyl ether (2.5 mL) maintaining a temperature below -45 ¡ãC. The mixture was allowed to warm to -20 ¡ãC and left to stir for 30 minutes. A solution of 2-chloro-N-methoxy-N-methyl acetamide (122 mg, 0.89 mmoles) in methyl tert- butyl ether (2.5 mL) was then added dropwise maintaining a temperature below -15 ¡ãC and the mixture allowed to stir for 20 minutes. The reaction was then quenched by the addition of saturated ammonium chloride solution (2.0 mL) and water (10.0 mL). The aqueous phase was extracted with methyl fert-butyl ether (2 x 10 mL) and the combined organic phases were dried (MgSC^), filtered and evaporated to give a pale orange solid. Purification by flash chromatography (isohexane/EtOAc, 95/5 to 90/10) gave title compound XVI as a beige solid (120 mg, 0.35 mmoles).1H NMR (500 MHz, CDC13) delta 7.75 (d, J= 8.5 Hz, 1H), 7.11 (d, J= 8.5 Hz, 1H), 5.46 (hept, J= 6.2 Hz, 1H), 4.79 (s, 2H), 1.50 (s, 9H), 1.47 (d, J= 6.2 Hz, 6H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 67442-07-3, its application will become more common.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; BARNWELL, Neil; CORNWALL, Philip; GILL, Duncan, Michael; HOWELL, Gareth, P.; MEADOWS, Rebecca, Elizabeth; MERIFIELD, Eric; MITCHELL, Christopher, William; MURUGAN, Andiappan; O’KEEFE, Philip; PATEL, Zakariya, Mohamed; ROSE, James, Barry; SINGLETON, John; WITHNALL, Jane; WO2012/156693; (2012); A1;,
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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. 53844-02-3, name is Benzyl (2-bromoethyl)carbamate, A new synthetic method of this compound is introduced below., Recommanded Product: 53844-02-3

The compound of Reference Example 55 (12.3 g) was dissolved in dimethylformamide (100 ml), and thereto were added cesium carbonate (15.3 g) and the compound of Reference Example 42 (8.75 g), and the mixture was vigorously stirred at 80C for 5 hours. The mixture was filtered to remove the cesium carbonate, and water was added to the filtrate, and extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid and saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and concentrated under reduced pressure. The obtained residue was purified by silica gel column (ethyl acetate/hexane=1:2) to give the title compound (10.7 g). MS (ESI+) 649 (M++1, 40%).

The synthetic route of 53844-02-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dainippon Sumitomo Pharma Co., Ltd.; EP2447264; (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. 22808-73-7, name is Methyl 4-sulfamoylbenzoate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H9NO4S

B. 4-(4-Oxo-2-m-tolyl-pentanoylsulfamoyl)-benzoic acid methyl ester. To a stirred solution of 4-sulfamoyl-benzoic acid methyl ester (6.01 g, 27.8 mmol), 4-oxo-2-m-tolyl-pentanoic acid (6.35 g, 30.7 mmol), N,N-diisopropylethylamine (12.2 mL, 69.5 mmol), and DMAP (5 mole %) in CH2Cl2 (275 mL) at rt under N2 was added bromo-tripyrrolidino-phosphonium hexafluorophosphate (PyBroP) (18.1 g, 38.9 mmol), and the reaction mixture was allowed to stir overnight. The mixture was diluted with 1 M HCl (100 mL) and CH2Cl2 (150 mL), and the layers were separated. The organic phase was washed with 1 M HCl (1*100 mL), 1N NaOH (1*100 mL) and brine (1*100 mL). The organic layer was dried over Na2SO4, and then filtered, and the solvent was removed under reduced pressure. Purification on silica gel (0-15% EtOAc in hexane) gave. 12.0 g (99%) of desired ester as a white solid. 1H NMR (400 MHz, CDCl3): 8.15 (d, J=8.6 Hz, 2H), 7.99 (d, J=8.6 Hz, 2H), 7.18 (t, J=7.6 Hz, 1H), 7.10 (d, J=7.6 Hz, 1H), 6.87 (m, 2H), 3.97 (s, 3H), 3.93 (dd. J=4.3 and 9.5 Hz, 1H), 3.29 (dd. J=9.5 and 18.1 Hz, 1H), 2.60 (dd. J=4.3 and 18.1 Hz, 1H), 2.28 (s, 3H), 2.07 (s, 3H).

The synthetic route of 22808-73-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Deng, Xiaohu; Mani, Neelakandha; Mapes, Christopher M.; US2006/4195; (2006); A1;,
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