Amides-buliding-blocks

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. 2603-10-3, name is Methyl N-Phenylcarbamate, A new synthetic method of this compound is introduced below., Quality Control of Methyl N-Phenylcarbamate

Aniline 4650 g, dimethyl carbonate 226.7 g,Zinc acetate 3.65 g in turn into the reactor,After replacing with nitrogen and pressurized to 0.2 Mpa, heated to 180 C,Reaction at this temperature for 5 h.After completion of the reaction, the temperature of the reactor was reduced to 80 C and constant temperature,To the autoclave, add 40 mL of concentrated hydrochloric acid,A constant-flow pump was added dropwise with an aqueous formaldehyde solution (40% by mass) at a dropping rate of 0.15 mL / min,The dropping time is 100 min. After completion of the dropwise addition, the reaction was continued at 80 C for 2 h.After completion of the reaction, the reaction solution was analyzed by high performance liquid chromatography,The yield of methyl 4,4′-diphenylmethane dicarbamate was 67%.

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; Research Institute of Nanjing Chemical Industry Group; ina Petroleum & Chemical Corporation; JIN, YUCUN; JIN H, ANQIANG; WU, QIJIAN; CHEN, YONGPING; LIU, ZHUO; HE, YUMIAO; (4 pag.)CN106543038; (2017); A;,
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Adding a certain compound to certain chemical reactions, such as: 97-35-8, name is 3-Amino-N,N-diethyl-4-methoxybenzenesulfonamide, 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 97-35-8, Product Details of 97-35-8

EXAMPLE 12 Synthesis of 2-hydroxy-3,6-bis(2-methoxy-5-diethylaminosulfonyl-aminocarbonyl)naphthalene STR22 3-Amino-4-methoxydiethylaminosulfonylbenzene (15.6 g), N-methyl-2-pyrrolidone (86.1 g) and toluene (34.3 g) were dissolved at room temperature and the acid chloride (5.4 g) obtained in Example 6 was gradually added, and then the mixture was amidated at 90 C. for 24 hours. After the reaction solution was cooled to 25 C. and filtered, toluene was distilled off under reduced pressure. Then, the solution was crystallized by using methanol (350.1 g). The resultant product was filtered and then dried to obtain 8.9 g of 2-hydroxy-3,6-bis(2-methoxy-5-diethylaminosulfonylphenyl-aminocarbonyl)naphthalene as a cream powdered crystal (DSC analysis value: 245.0 C.). An infrared spectrum (KBr method) of this compound is shown in FIG. 12.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Kabushiki Kaisha Ueno Seiyaku Oyo Kenkyujo; US5786523; (1998); A;,
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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. 830-43-3, name is 4-(Trifluoromethyl)benzenesulfonamide, A new synthetic method of this compound is introduced below., Quality Control of 4-(Trifluoromethyl)benzenesulfonamide

General procedure: All solid chemicals used were dried in vacuum over P2O5 overnight.The acid derivative and CDI were dissolved in dry THF underN2 atmosphere and the mixture was allowed to stir at 66-68 C for2 h. The sulfonamide and DBU dissolved in THF were added to thereaction mixture and stirring was continued at room temperature(4 h-overnight).Method B1: The solvent was removed in vacuo, water was addedand pH was adjusted to 2 by addition of 1 M HCl aq. The aqueousphase was extracted with EtOAc (2 40 ml), dried with MgSO4, filteredand evaporated in vacuo. For most of the compounds, a silicagel column was first run, followed by purification on aluminumoxide.

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; Belfrage, Anna Karin; Abdurakhmanov, Eldar; Akerblom, Eva; Brandt, Peter; Oshalim, Anna; Gising, Johan; Skogh, Anna; Neyts, Johan; Danielson, U. Helena; Sandstroem, Anja; Bioorganic and Medicinal Chemistry; vol. 24; 12; (2016); p. 2603 – 2620;,
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Adding a certain compound to certain chemical reactions, such as: 618-48-4, name is 3-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 618-48-4, SDS of cas: 618-48-4

General procedure: DDQ (20 mol%, 9.08 mg, 0.04 mmol) and BPO (20 mol%,9.69 mg, 0.04 mmol) were added to a mixture of 1,3-diarylpropene1 (0.24 mmol) and substrate 2 (0.2 mmol) in CH3NO2 (1 mL). Thereaction was carried out at 100 C under an oxygen atmosphere(oxygen balloon) for 24 h. The resulting mixture was purified by flashcolumn chromatography on silica gel (petroleum ether:ethyl acetate =10:1-20:1) to give the desired pure product 3a-k.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Cheng, Dongping; Zhou, Xiayi; Yuan, Kun; Yan, Jizhong; Journal of Chemical Research; vol. 40; 3; (2016); p. 127 – 129;,
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Reference of 50667-69-1, These common heterocyclic compound, 50667-69-1, name is 2,2,2-Trifluoro-N-(hydroxymethyl)acetamide, 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 solution of 2,3,4,5-tetrachloro-6-(2-(4′-carboxyphenyl)-7-chloro-6-hydroxy-3-oxo-3H-xanthen-9-yl)-benzoic acid (200 mg, 0.32 mmol, as prepared in Example 1), and N-(hydroxymethyl) trifluoroacetamide (44 mg, 0.31 mmol, Lancaster, Inc) in sulfuric acid (3 mL) was stirred at room temperature over a period of 16 h then poured into crushed ice (25 g). The crude product was extracted with EtOAc (250 mL) and the combined organic portions were washed with water (150 mL) and saturated NaCl (150 mL), dried (MgSO4) and concentrated. Purification via column chromatography (silica gel, 60 g, 1/1 EtOAc/hexanes 1% AcOH) gave the title compounds as a mixture (105 mg, 62%).

The synthetic route of 50667-69-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; O’Neill, Roger; Fisher, Peter V.; US2004/73014; (2004); A1;,
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316146-27-7, name is N-(4-Bromophenyl)-3-phenylpropanamide, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C15H14BrNO

Intermediate 2 The reaction was carried out twice . POCI3 (1.225 mol) was added dropwise at 10 0C to DMF (0.525 mol) . Then intermediate 1 (0.175 mol) was added at room temperature. The mixture was stirred overnight at 80 0C, poured out on ice and extracted with CH2CI2 . The organic layer was dried (MgSO/t), filtered, and the solvent was evaporated, yielding 77.62 g (67percent) of intermediate 2. The product was used without further purification.

The synthetic route of 316146-27-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2007/14934; (2007); A2;,
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Some common heterocyclic compound, 917342-29-1, name is tert-Butyl (trans-4-(2-hydroxyethyl)cyclohexyl)carbamate, molecular formula is C13H25NO3, 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: tert-Butyl (trans-4-(2-hydroxyethyl)cyclohexyl)carbamate

The compound 20 (3.40 g, 13.97 mmol) was dissolved in dichloromethane (34 mL). To the solution was added 4 mol/L hydrochloric acid (dioxane solution, 34.9 mL, 140 mmol). The mixture was stirred at room temperature for 3 hours. To the mixture, methanol (5 mL) was added and the mixture was stirred at room temperature for 1 hour. The solvent was evaporated under reduced pressure to give a compound 21 as a crude product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 917342-29-1, its application will become more common.

Reference:
Patent; Shionogi & Co., Ltd.; TOBINAGA, Hiroyuki; MASUDA, Koji; KASUYA, Satoshi; INAGAKI, Masanao; YONEHARA, Mitsuhiro; MASUDA, Manami; (289 pag.)US2019/161501; (2019); A1;,
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Application of 71999-74-1, 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. 71999-74-1, name is N-Boc-2-chloroethylamine belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 142 Synthesis of the compound of the following formula (E-51) which has a substituent(s) of Example 142 of Table 23: N-(2,6-dichlorobenzoyl)-4-[6-(2-dimethylaminoethoxy)-1-methyl-2,4-quinazol ine-dione-3-yl]-L-phenylalanine t-Butyl 2-chloroethylcarbamate (157 mg), DMF (3 mL) and potassium carbonate (1384 mg) were added to the compound of Example 154 (450 mg) and stirred at 90 C. overnight. The mixture was extracted with ethyl acetate and treated in accordance with the ordinary method. The obtained crude material was dissolved in 4N hydrogen chloride dioxane solution (2 mL) and stirred at room temperature for 2 hours. After removing the solvent, the residue was purified with high performance liquid chromatography (water/acetonitrile, each containing 0.1% TFA) to obtain 350 mg of a purified material. Acetonitrile (5 mL), formalin (37 muL), acetic acid (26 muL) and triacetoxy sodium boron (98 mg) were added to the obtained purified material (170 mg) and stirred at room temperature for 2 hours. After removing the solvent, the residue was purified with high performance liquid chromatography (water/acetonitrile, each containing 0.1% TFA) to obtain 150 mg of a purified material. 4N hydrogen chloride dioxane solution (1 mL) and water (200 muL) were added to the obtained purified material (20 mg) and stirred at 90 C. for 2 hours. After removing the solvent, the residue was purified with high performance liquid chromatography (water/acetonitrile, each containing 0.1% TFA) to obtain 11 mg of a purified material. MS(ESI MH+): 599 Example 155 Synthesis of the Compound of the Following Formula (E-51) which has a Substituent(s) of Example 155 of Table 25: N-(2,6-dichlorobenzoyl)-4-[6-(2-dimethylaminoethoxy)-1-methyl-2,4-quinazol ine-dione-3-yl]-L-phenylalanine isopropylester t-Butyl 2-chloroethylcarbamate (157 mg), DMF (3 mL) and potassium carbonate (1384 mg) were added to the compound of Example 154 (450 mg) and stirred at 90 C. overnight. The mixture was extracted with ethyl acetate and treated in accordance with the ordinary method. The obtained crude material was dissolved in 4N hydrogen chloride dioxane solution (2 mL) and stirred at room temperature for 2 hours. After removing the solvent, the residue was purified with high performance liquid chromatography (water/acetonitrile, each containing 0.1% TFA) to obtain 350 mg of a purified material. Acetonitrile (5 mL), formalin (37 muL), acetic acid (26 muL) and triacetoxy sodium boron (98 mg) were added to the obtained purified material (170 mg) and stirred at room temperature for 2 hours. After removing the solvent, the residue was purified with high performance liquid chromatography (water/acetonitrile, each containing 0.1% TFA) to obtain 150 mg of the intended compound. MS(ESI MH+): 641

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-Boc-2-chloroethylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Ajinomoto Co., Inc.; US2005/222141; (2005); A1;,
Amide – Wikipedia,
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Synthetic Route of 96-30-0,Some common heterocyclic compound, 96-30-0, name is 2-Chloro-N-methylacetamide, molecular formula is C3H6ClNO, 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 3. Preparation of 2-[4-(5-cyano-2-methoxyphenoxy)piperidin-l-yl]-JV- methylacetamide (Compound (V)).; Compound (VI) (28.36 g, 95.82 mmoles), 2-chloro-N- methylacetamide (12.37 g, 114.98 mmoles) and potassium carbonate (33.11 g, 239.55 mmoles) were suspended in acetonitrile (161.36 g). The reaction mixture was heated at reflux for 3 hours. The reaction mixture was cooled to 200C and water (386.26 g) was charged. The reaction was heated to 75C and the volume reduced by distillation. Upon cooling crystallisation occurred. The resulting solid was isolated by filtration, washed twice with water (77.25 g and 128.75 g) and then dried to give compound (V) (27.95 g, 94% yield); 1H NMR (400 MHz, DMSO-J6) delta ppm 1.68 (m, 2 H) 1.91 (m, 2 H) 2.29 (m, 2 H) 2.61 (d, J=4.7 Hz, 3 H) 2.67 (m, 2 H) 2.88 (s, 2 H) 3.83 (s, 3 H) 4.41 (tt, J=8.3, 4.0 Hz, 1 H) 7.11 (d, J=8.4 Hz, 1 H) 7.40 (dd, J=8.4, 1.9 Hz, 1 H) 7.47 (d, J=I.9 Hz, 1 H) 7.68 (q, J=4.7 Hz, 1 H); Mass Spectrum: m/z (M + H)+ 304.2.

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-methylacetamide, its application will become more common.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; BOARDMAN, Kay, Alison; CUNNINGHAM, Oliver, Robert; GOUNDRY, William; LAFFAN, David, Dermot, Patrick; WO2010/122340; (2010); A2;,
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Some common heterocyclic compound, 143557-91-9, name is tert-Butyl 3-endo-3-hydroxy-8-azabicyclo[3.2.1]octane-8-carboxylate, molecular formula is C12H21NO3, 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. HPLC of Formula: C12H21NO3

Compound I (4.23 g) was dissolved in DMF (100 mL), and thereto were added benzyl bromide (3.32 mL) and sodium hydride (1.62 g), and the mixture was stirred at room temperature overnight. To the reaction mixture was added water, and the mixture was extracted with diisopropylether. The organic layer was dried over sodium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=3/1) to give the title compound II (4.98 g).1H-NMR (CDCl3) delta1.47 (s, 9H), 1.93-2.05 (m, 6H), 2.13-2.19 (m, 2H), 3.72 (m, 1H), 4.12-4.26 (m, 2H), 4.49-4.50 (m, 2H), 7.26-7.30 (m, 1H), 7.32-7.41 (m, 4H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 143557-91-9, its application will become more common.

Reference:
Patent; DAINIPPON SUMITOMO PHARMA CO., LTD.; US2012/225876; (2012); A1;,
Amide – Wikipedia,
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