Month: August 2021

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. 85006-25-3, name is tert-Butyl (tert-butoxycarbonyl)oxycarbamate, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 85006-25-3

General procedure: Method D: To a solution of acyl Meldrum?s acid (1.69mmol, 1.8equiv) in dry toluene (4.5mL) at room temperature was added N,O-bis(tert-butoxycarbonyl)hydroxylamine (219mg, 0.938mmol, 1.0equiv), and the reaction mixture was immersed in an oil bath preheated to 90C. The reaction was monitored for the complete consumption of N,O-bis(tert-butoxycarbonyl)hydroxylamine. Leaving the reaction for longer time can lead to loss in yield and competing side reactions. After concentration in vacuo, the residue was purified on silica gel chromatography using 5% ethyl acetate in hexane to yield beta-keto hydroxamic acid (12a, d, f-i, l, p) as colorless oil.

According to the analysis of related databases, 85006-25-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Verma, Astha; Wong, Dawn M.; Islam, Rafique; Tong, Fan; Ghavami, Maryam; Mutunga, James M.; Slebodnick, Carla; Li, Jianyong; Viayna, Elisabet; Lam, Polo C.-H.; Totrov, Maxim M.; Bloomquist, Jeffrey R.; Carlier, Paul R.; Bioorganic and Medicinal Chemistry; vol. 23; 6; (2015); p. 1321 – 1340;,
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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. 29579-11-1, name is 2-(Benzyloxy)benzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 29579-11-1

General procedure: The appropriate amide 32a-p, benzhydrazide (40a), or p-toluenesulfonylhydrazide (43a) (1.0 mmol, 1.0 equiv) was placed in a SchlenkKjeldahl reaction flask and the flask was evacuated/argon re-filledthree times. Subsequently, anhyd CH2Cl2 (25 mL) was added and themixture was stirred at r.t. for 10 min before dropwise addition of oxalylchloride (3.0 mmol, 3.0 equiv) followed. The reaction mixturewas then stirred at reflux for 2.5-3.0 h before cooling to r.t. and thesolvent was evaporated in vacuo. Subsequently, the appropriate nucleophile32, 34, 36, 38, 40, 42, 43, or 45 (1.1-1.25 mmol, 1.1-1.25equiv) was rapidly added and the flask was evacuated/argon re-filledbefore anhyd toluene (12 mL) was added. The reaction mixture wasthen stirred at reflux for 2.5-3 h before cooling to r.t. and concentrationto about 1/3 of the initial volume on rotavapor. Hexane was addedto the residue and the obtained precipitate (often sonicated) wascollected by filtration under reduced pressure to yield the crudeproduct. When necessary, the isolated material was purified either bycrystallization from MeOH or flash chromatography on silica gel withhexane-EtOAc as the eluent.

The synthetic route of 29579-11-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hernandez, Anolan Garcia; Grooms, Gregory M.; El-Alfy, Abir T.; Stec, Jozef; Synthesis; vol. 49; 10; (2017); p. 2163 – 2176;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 177906-48-8 as follows. Application In Synthesis of trans-N-Boc-1,4-cyclohexanediamine

To a solution of 6-bromo-2-fluoro-8-(trifluoromethyl)quinazoline (0.4 g, 1.3 mmol) in n-BuOH (20.0 mL) were added tert-butyl N-(4-aminocyclohexyl)carbamate (349 mg, 1.6 mmol) and DIEA (350 mg, 2.7 mmol, 472.3 uL). The mixture was stirred at 100C for 12 h. The mixture was cooled to 25C and filtered. The cake was washed with Petroleum ether (50.0 mL) to afford tert-butyl ((lr,4r)-4-((6-bromo-8-(trifluoromethyl)quinazolin-2- yl)amino)cyclohexyl) carbamate (0.5 g, 1.0 mmol, 74.6% yield). M+H+ = 491.2 (LCMS).

According to the analysis of related databases, 177906-48-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; QUENTIS THERAPEUTICS, INC.; VACCA, Joseph P.; LI, Dansu; BETTIGOLE, Sarah; (184 pag.)WO2018/222918; (2018); A1;,
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Some common heterocyclic compound, 445-28-3, name is 2-Fluorobenzamide, molecular formula is C7H6FNO, 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. Computed Properties of C7H6FNO

Example 57 In analogy to example 47, on reaction of 7-iodo-2-methyl-4-pyrrolidin-1-yl-quinoline with 2-fluorobenzamide there was obtained: 2-fluoro-N-(2-methyl-4-pyrrolidin-1-yl-quinolin-7-yl)-benzamide as light yellow solid. ISP mass spectrum, m/e: 350.3 (M+1 calculated for C21H20FN3O: 350).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 445-28-3, its application will become more common.

Reference:
Patent; Mattei, Patrizio; Mueller, Werner; Neidhart, Werner; Nettekoven, Matthias Heinrich; Pflieger, Philippe; US2003/153553; (2003); 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. 402-46-0, name is 4-Fluorobenzenesulfonamide, A new synthetic method of this compound is introduced below., Product Details of 402-46-0

General procedure: To a round-bottom flask (500 mL) that contained a solution of aryl sulfonamide (6 mmol), 4-dimethyaminopyridine (DMAP, 13 mmol), and 1-[3-(dimethyamino)-propyl]-3-ethylcarbodiimide hydrochloride (EDCI, 13 mmol) in CH2Cl2 (150 mL) was added the synthesized phenylacetic acid (6 mmol) at room temperature. The resulting mixture was stirred at room temperature for 12 h, then cooled to 5 C, and acidified to pH 1 with addition of HCl aqueous solution (10%), which was followed by extraction with CH2Cl2/MeOH (9:1, 3 × 100 mL). The combined organic layers were washed with H2O and brine, dried over Na2SO4, and concentrated in vacuo. The residue was subjected to silica gel chromatography or crystallization if necessary to afford the compounds (20-44) (Scheme 2).

The synthetic route of 402-46-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Luo, Yin; Li, Yao; Qiu, Ke-Ming; Lu, Xiang; Fu, Jie; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry; vol. 19; 20; (2011); p. 6069 – 6076;,
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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. 683-57-8, name is 2-Bromoacetamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C2H4BrNO

(0.86 g, 10 mmol) piperazine was dissolved in THF and (2.76 g, 20 mmol) potassium carbonate was added and mixture was stirred at room temperature for 20 min and then (2.90 g, 21mmol) 2-bromoacetamine was added. The mixture was stirred for 15 h and the completion of the reaction was monitored by TLC analysis and upon the completion, the solid was filtered with sintered glass funnel. The filtrate was evaporated by rotary evaporator and the residue was dried in vacuum desiccator. The best yields of the desired products were obtained when the reaction was carried out in THF at room temperature with a 1:2 mole ratio of the reagents. Formation of HBr is eliminated with subsequent treatment of this salt with saturated aqueous sodium carbonate. The white crystals were obtained. The compound was characterized using different spectroscopic techniques, including IR, NMR and MS, elemental analyses. Reaction scheme is given in Scheme 1. (0005) Yield: 77%, 1.6g. Anal. calcd. for C8H16N4O2, (200.24g/mol): C 47.99%; H 8.05%; N 27.98%. Found: C 47.83%; H 8.14%; N 27.82%. FT-IR (KBr, cm-1): 1675 nu(C=0, amide), 3323, 3213, 3146 nu(N-H). 1H NMR (delta, ppm, CD3OD): 7.33 (NH2, s, 4H), 3.91(s, CH2-N, 4H), 3.50-3.60 (d t, piperazine ring, 8H), 13C NMR (delta, ppm, CDCl3): 167.89 (C=O), 56.79 (CH2-N, 2C), and 49.74 (piperazine ring, 4C). GS MS (E, m/z): [M] +, 200.99.

The synthetic route of 683-57-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kacan, Mesut; Turkyilmaz, Murat; Karabulut, Ferhat; Altun, Ozlen; Baran, Yakup; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 118; (2014); p. 572 – 577;,
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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. 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;,
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Application of 142733-64-0, These common heterocyclic compound, 142733-64-0, name is tert-Butyl (cis-3-(hydroxymethyl)cyclobutyl)carbamate, 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.

Under nitrogen protection,Compound 3-Boc aminocyclobutylmethanol (83f) (350.0 mg, 1.7 mmol)And triethylamine (528.0 mg, 5.2 mmol) was dissolved in 10 mL of dichloromethane.Under ice water bath, methylsulfonyl chloride (219.0 mg, 1.9 mmol) was added dropwise.Stir at room temperature for 3 h.Dichloromethane and 0.2 N of dilute hydrochloric acid were added and extracted.The organic layer was washed twice with brine, dried and dried.The compound 3-((tert-butoxycarbonyl)amino)cyclobutyl)methyl methanesulfonate (83 g) (330.0 mg, 1.2 mmol)The next reaction was directly administered, and the yield was 67.9%.

The synthetic route of 142733-64-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chengdu Haichuang Pharmaceutical Co., Ltd.; Du Wu; Wen Kun; Ai Chaowu; He Jinyun; Li Xinghai; Chen Yuanwei; (28 pag.)CN109988120; (2019); A;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 749927-69-3 as follows. COA of Formula: C8H7BrFNO

A mixture of 4-bromo-2-fluoro-N-methylbenzamide (900 mg, 3.9 mmol), 5-(4,4,5,5- tetramethyl-l,3,2-dioxaborolan-2-yl)pyrimidin-2-amine (710 mg, 3.2 mmol), tetrakis(triphenylphosphine)palladium (100 mg, 0.1 mmol) and potassium carbonate (1.3 g, 9.7 mmol) in toluene (6.0 mL) and ethanol (3.0 mL) and water (3.0 mL) was heated at 110 0C for 2 hours. After cooling to RT, the reaction mixture was quenched with water and extracted with diethyl ether. The solid was filtered and washed with water and diethyl ether to afford the desired product (720 mg).

According to the analysis of related databases, 749927-69-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; INCYTE CORPORATION; ZHUO, Jincong; METCALF, Brian; WO2008/64157; (2008); A1;,
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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;,
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