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. 6973-09-7, name is 5-Amino-2-methylbenzenesulfonamide, A new synthetic method of this compound is introduced below., Safety of 5-Amino-2-methylbenzenesulfonamide

Example 4b: Synthesis of Pazopanib Hydrochloride (0040) To a suspension of N-(2-chloropyrimidin-4-yl)-N-2,3-trimethyl-2H-indazol-6-amine (90 g, 0.312 mol) and 5-amino-2-methyl benzene sulfonamide (64.07 g, 0.344 mol) in isopropyl alcohol (900 mL) was added 4M hydrochloric acid solution in isopropyl alcohol (1.56 mL, 6.25 mol). The reaction mixture was heated to reflux temperature for 10 hours to 12 hours. The reaction mixture was cooled to 25 C. The reaction mixture was further stirred at 25 C. to 30 C. for 30 minutes, then the solid was filtered. The wet solid was washed with isopropyl alcohol (180 mL×2), and then dried under vacuum at 45 C. to 50 C. for 12 hours to afford the hydrochloride salt of 5-({4-[(2,3-dimethyl-21-I-indazol-6-yl)(methyl) amino] pyrimidin-2-yl} amino-Z-methylbenzene sulfonamide as a light brown solid. Yield: 97% w/w.

The synthetic route of 6973-09-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sun Pharmaceutical Industries Limited; KUMAR, Rajesh; GIRI, Prabhat; BARMAN, Dhiren C.; NATH, Asok; PRASAD, Mohan; (5 pag.)US2015/329526; (2015); A1;,
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Application of 683-57-8, The chemical industry reduces the impact on the environment during synthesis 683-57-8, name is 2-Bromoacetamide, I believe this compound will play a more active role in future production and life.

Example 25; 2-[4-({|2-(trifluoroniethyl)phenyl]sulfonyl}amino)piperidin-l-yl]acetamide; [0234] To a suspension of N-piperidin-4-yl-2-(trifluoromethyl)benzenesulfonamide hydrochloride salt, example 3, (74 mg, 0.21 mmol) in acetone was added potassium iodide (catalytic amount) and bromoacetamide (33 mg, 0.23 mmol). The reaction mixture was heated (500C, 16 h) and monitored by LCMS. The solvent was removed in vacuo and water was added. The product was extracted with ethyl acetate and concentrated to dryness. The crude residue was purified by flash chromatography using asolvent system comprised of dichloromethane and 10% methanolic dichloromethane (0 to 80%). The isolated free base was dissolved in ethyl acetate and treated with HCl gas to afford the hydrochloride salt of 2- [4-({[2-(trifluoromethyl)phenyl]sulfonyl}amino)piperidin-l-yl]acetamide (72 mg, 85%).[0235] MS (ESI+) m/z 366;HPLC purity 100.0%, Rtau 4.6 minutes;HRMS: calculated for C4H18F3N3O3S + H+, 366.10937; found (ESI, [MH-H]+), 366.1075;

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-Bromoacetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WYETH; WO2008/61016; (2008); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2895-21-8, name is N-Isopropyl-2-chloroacetamide, 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 2895-21-8, Application In Synthesis of N-Isopropyl-2-chloroacetamide

A mixed solution of the compound 1 (120 mg), the compound 2 (123 mg), and sodium carbonate (96 mg) in acetonitrile (5 mL) was stirred for 22 hours at 50C under argon atmosphere. The reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed with water and saturated brine, and dried over Chem Elut (registered trademark). The solvent was distilled off under reduced pressure, and the resultant residue was purified by silica gel column chromatography (eluent: chloroform-ammonia water (10% methanol solution) = 90:10). The resultant residue was triturated with a mixed solvent of hexane-ethyl acetate to give the compound 3 (95 mg) as a pale yellow solid. MS (APCI) 365 [M+H]+

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

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; SAKAKIBARA, Ryo; USHIROGOCHI, Hideki; SASAKI, Wataru; ONDA, Yuichi; YAMAGUCHI, Minami; AKAHOSHI, Fumihiko; (69 pag.)EP3381904; (2018); 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. 39549-79-6, name is 2-Amino-4-methylbenzamide, A new synthetic method of this compound is introduced below., Quality Control of 2-Amino-4-methylbenzamide

General procedure: Sodium hydrogen sulfite (4 mmol) was added to a solution of anthranilamide 1 (2 mmol) and benzaldehyde 2 (2 mmol) in N,N- dimethylacetamide (5 mL). The mixture was heated under continuous stirring at 150 o C for 2-3 h and poured into ice water. The precipitate was then filtered, washed with water followed byethanol, and dried to yield the 2-arylquinazolinones 3-31.#10;#10;

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; Khadka, Daulat Bikram; Tran, Giap Huu; Shin, Somin; Nguyen, Hang Thi Minh; Cao, Hue Thi; Zhao, Chao; Jin, Yifeng; Van, Hue Thi My; Chau, Minh Van; Kwon, Youngjoo; Le, Thanh Nguyen; Cho, Won-Jea; European Journal of Medicinal Chemistry; vol. 103; (2015); p. 69 – 79;,
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Adding a certain compound to certain chemical reactions, such as: 57957-24-1, name is N-(1-Phenylvinyl)acetamide, 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 57957-24-1, Safety of N-(1-Phenylvinyl)acetamide

General procedure: A reaction tube was charged with N-acetylenamide 1a (100 mg, 0.636 mmol), alkyne 2a (124 mg, 0.699 mmol), Cu(OAc)2.H2O (126 mg, 0.636 mmol), KPF6 (23.4 mg, 0.127 mmol) and [RuCl2(p-cymene)]2 (7.8 mg, 0.0127 mmol). To that, DME or water (3 mL) was added by syringe. The reaction mixture was stirred at 110 C under N2 as indicated time in the table 1.The reaction mixture was cooled down to rt, diluted with 10 mL of DCM. The mixture was then filtered through Celite. The combined organic portion was washed with water, then dried over MgSO4 and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel with hexane/ethyl acetate as eluent to yielded the desired pyrrole 3a (202 mg, 0.605 mmol) in 95% yield. Products obtained in this work were characterized by spectral methods particularly with 1H, 13C NMR, and ESI-Mass analyses, further, the data were compared with those reported.

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-(1-Phenylvinyl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Murugan, Kaliyappan; Liu, Shiuh-Tzung; Tetrahedron Letters; vol. 54; 21; (2013); p. 2608 – 2611;,
Amide – Wikipedia,
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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. 22961-58-6, name is 5-Amino-2-methoxybenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 5-Amino-2-methoxybenzamide

EXAMPLE 67 3′-Methoxy-2′-methylcarbamoyloxanilic acid ethyl ester. 72 Slow addition of 4.98 g. (0.03 mole) of 5-amino-o-anisamide to a mixture of 57% NaH (1.32 g., 0.0315 mole) in 50 ml. dimethylformamide was carried out at room temperature. After the evolution of H2 ceased, the mixture was cooled to 3 C. and 2.06 ml. (0.033 mole) of methyliodide was slowly added at 3-5 C. The temperature was allowed to go up to room temperature and stir for 2 hours. The mixture was concentrated, the residue extracted into ethylacetate-water, the mixture was basified, and the ethylacetate layer was washed with water, brine and dried. Concentration gave a tan solid that was crystallized (ethanol), giving 0.45 g. (8%) of 6-amino-N-methyl-o-anisamide mp. 186-189 C.

The synthetic route of 22961-58-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; American Home Products Corporation; US4054661; (1977); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 17641-08-6,Some common heterocyclic compound, 17641-08-6, name is 2-Chloro-N-(3-methoxyphenyl)acetamide, molecular formula is C9H10ClNO2, 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: The oxime 6 or 8 (0.7 mmol) and K2CO3(0.116 g, 0.84 mmol) were taken in dry DMF (5 mL), cooled to 0 Cand stirred for 30 min, then N-substituted acetamide (0.77 mmol)was added. The total reaction mixture was stirred at room temperature for 12-20 h. The reaction was monitored by TLC and after completion of the reaction, treated with ice cold water. Aqueous solution was extracted thrice with ethylacetate, combined extracts were washed with water till washings are neutral to pH, dried over anhydrous sodium sulfate and concentrated. The residue was purifiedby passing through a column packed with silica gel using petroleum ether/EtOAc (8:2) as eluent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-N-(3-methoxyphenyl)acetamide, its application will become more common.

Reference:
Article; Gannarapu, Malla Reddy; Vasamsetti, Sathish Babu; Punna, Nagender; Royya, Naresh Kumar; Pamulaparthy, Shanthan Rao; Nanubolu, Jagadeesh Babu; Kotamraju, Srigiridhar; Banda, Narsaiah; European Journal of Medicinal Chemistry; vol. 75; (2014); p. 143 – 150;,
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Application of 39549-79-6,Some common heterocyclic compound, 39549-79-6, name is 2-Amino-4-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: A 12mL vial was charged with MCM-41-2P-Pd(OAc)2 (2molpercent), 2-aminobenzamide (1mmol), aryl iodide (1mmol) (if solid) and a stirring bar. Then, DMF (2mL), aryl iodide (1mmol) (if liquid) and DBU (2mmol) were injected by syringe under an argon atmosphere. The vial was placed in an alloy plate, which was transferred into a 300mL Parr Instruments 4560 series autoclave under an argon atmosphere. After flushing the autoclave three times with CO, a pressure of 10bar CO was fixed at ambient temperature. The autoclave was heated for 20hat 120°C. After completion of the reaction, the autoclave was cooled to room temperature and the pressure was released carefully. The reaction mixture was diluted with ethyl acetate (10mL) and filtered. The palladium catalyst was washed with distilled water (2×5mL) and acetone (2×5mL), and reused in the next run. The filtrate was concentrated in vacuo and the pure product was isolated by either washed with water, ethyl acetate and finally hexane or recrystallization from MeOH.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Amino-4-methylbenzamide, its application will become more common.

Reference:
Article; You, Shengyong; Huang, Bin; Yan, Tao; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 875; (2018); p. 35 – 45;,
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Related Products of 6331-71-1, A common heterocyclic compound, 6331-71-1, name is 4-Amino-N,N-dimethylbenzamide, molecular formula is C9H12N2O, 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.

The triflate E-7c (22.1 mg, 0.05720 mmol, 1.0 eq) was combined with 4-(amino)-N,N- dimethyl benzamide (11.27 mg, 0.06864 mmol, 1.2 eq), palladium(II)acetate (1.28 mg, 0.005720 mmol, 0.1 eq), Xantphos (6.62 mg, 0.01144 mmol, 0.2 eq) and potassium carbonate (180.9 mg, 1.1440 mmol, 20 eq). To this was added degassed 1,4-dioxane (3.0 mL). The vessel was then sealed, evacuated, and flushed with N2. The reaction was heated to 100 0C and stirred for 18 hours. The reaction was then cooled. The solvent was removed under reduced pressure. The residue was taken up in 4 mL of methanol and filtered through a 0.45 micron syringe filter. Purification by reverse phase preparatory HPLC provided Compound [103]. Data for Compound [103]: LCMS m/e 401; 1H NMR (400 MHz, Methanol-^) delta ppm 1.72 (s, 3 H), 1.76 (s, 3 H), 3.14 (s, 6 H), 5.10 – 5.19 (m, 1 H), 7.40 – 7.46 (m, 1 H), 7.46 – 7.53 (m, 2 H), 7.81 – 7.91 (m, 2 H), 8.34 – 8.44 (m, 1 H), 8.47 – 8.57 (m, 1 H), 9.11 – 9.18 (m, 2 H), 9.37 – 9.45 (m, 1 H).

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; MERCK SHARP & DOHME CORP.; BANYU PHARMACEUTICAL CO., LTD.; GOTO, Yasuhiro; SAGARA, Takeshi; FAN, Weiming; HAXELL, Thomas, F. N.; JENKS, Matthew, G.; MALASKA, Michael, J.; MOORE, Joseph, A., III; OUVRY, Gilles; PANDI, Bharathi; PEEL, Michael, R.; STEWARD, Kimberly, M.; WO2010/42337; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 2227-79-4, name is Benzothioamide, A new synthetic method of this compound is introduced below., Recommanded Product: Benzothioamide

The bottle to the three port by adding benzthioamides (20.00 g, 0 . 146 mol), methanol 200 ml, 1,3-dichloroacetone (22.21 g, 0 . 157 mol), heated up to reflow, reflux reaction 3 hours. Lowering the temperature to after the end of the reaction 30 C the following, the reaction solution into 50 ml of water, with 3×50 ml of ethyl acetate extraction, the resulting organic phase with saturated aqueous solution of sodium bicarbonate (50 ml), saturated sodium chloride aqueous solution after washing (50 ml), dried with anhydrous magnesium sulfate, after concentrating under reduced pressure, the residue by column chromatography separation (showering liquid: ethyl acetate: petroleum ether = 1:10) shall be 21.00 g 4 – (chloro methyl) – 2-phenyl-thiazole, decadent oil, yield: 69%.

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; SINOCHEM CORP, Shenyang Research Institute OfChemical Industry Co., Ltd .; YANG, HUIBIN; LI, BIN; SONG, YUQUAN; LIU, HONGYI; WANG, BIN; ZHANG, YU; FENG, CONG; TONG, YICHUN; CHU, YANFENG; CHEN, LIN; YU, HAIBO; (17 pag.)CN103833667; (2016); B;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics