Author: tianli

Reference of 49805-30-3,Some common heterocyclic compound, 49805-30-3, name is 2-Azabicyclo[2.2.1]hept-5-en-3-one, molecular formula is C6H7NO, 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.

1.6. Preparation of a (+-)-1-amino-4-(hydroxymethyl)-2-cyclopentene in an alcohol/ether mixture A 10 ml round-bottom flask was charged under at inert-gas atmosphere with 0.5 g (4.6 mmol) of (+-)-2-azabicyclo[2.2.1]hept-5-en-3-one and 0.59 g (18.4 mmol) of methanol in 7.5 ml of dioxane (abs.). 0.21 g (9.2 mmol) of lithium borohydride were added, and the mixture was heated for 4 h at 60 C. The mixture was then cooled to 5 C. using an ice/waterbath, and about 10 ml of semi-concentrated HCl was carefully added to the reaction mixture (vigorous reaction, gas evolution), as a result of which a yellowish clear solution formed. This solution was analyzed directly by a quantitative ion-chromatographic method It contained 0.60 mmol (13.1%) of (+-)-2-azabicyclo[2.2.1]hept-5-en-3-one (determined as HCl salt of the corresponding amino acid, which is the acidic hydrolysis product of (+-)-2-azabicyclo-[2.2.1]hept-5-en-3-one) and 3.06 mmol of product, corresponding to a yield of 66.8%, aminoalcohol

The synthetic route of 49805-30-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lonza AG; US2002/10360; (2002); A1;,
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. 115643-59-9, name is 2-Amino-6-fluorobenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 2-Amino-6-fluorobenzamide

Step 1 To a solution of 2-amino-6-fluorobenzamide (3.80 g, 24.7 mmol) and triethylamine (2.99 g, 29.6 mmol) in THF (50 mL) was added dropwise ethyl chloroglyoxylate (3.70 g, 27.1 mmol) under ice-cooling, and the mixture was stirred at room temperature for 3 hr. The mixture was partitioned between ethyl acetate and water, and the organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was suspended in ethanol, and the insoluble material was collected by filtration to give ethyl ((2-(aminocarbonyl)-3-fluorophenyl)amino)(oxo)acetate as a white powder (4.95 g, 79%).

The synthetic route of 115643-59-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP1953148; (2008); A1;,
Amide – Wikipedia,
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Synthetic Route of 177906-48-8, The chemical industry reduces the impact on the environment during synthesis 177906-48-8, name is trans-N-Boc-1,4-cyclohexanediamine, I believe this compound will play a more active role in future production and life.

Method E The reaction mixture of Core C (1.00 eq) and amine n (4.00 eq) in DMSO (8 mL) was stirred at 160 C for 3 h. The reaction mixture was cooled to rt and poured onto ice-H20 (20 mL). The aqueous layer was extracted with EA (50 mL*3). The combined organic layers were washed with brine (50 mL*3), dried over Na2S04, filtered and concentrated. The residue was purified by column chromatography to give A-n. Step 1: Compound 27_2 was made according to the procedure descibed in method E with amine-27 (1.0 eq) and DIEA (10 eq) at 160C for 6 h and it was obtained as a yellow solid after purification by prep HPLC (TFA). Yield: 41.1% NMR (CDCb, 400 MHz) delta 8.18 (d, / = 5.2 Hz, 1H), 7.83 (s, 1H), 6.71 (d, / = 5.6 Hz, 1H), 4.87 (s, 1H), 4.41 (s, 1H), 3.89 – 3.82 (m, 4H), 3.49 (s, 1H), 3.19 (d, / = 6.3 Hz, 2H), 2.19 – 2.05 (m, 4H), 1.46 (s, 9H), 1.35 – 1.29 (m, 7H), 1.26 (m, 2H), 1.23 (m, 2H), 0.50 – 0.46 (m, 2H), 0.26 – 0.24 (m, 2H)

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, trans-N-Boc-1,4-cyclohexanediamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; YISSUM RESEARCH DEVELOPMENT COMPANY OF THE HEBREW UNIVERSITY OF JERUSALEM LTD; BEN NERIAH, Yinon; BRACHYA, Guy; BURSTAIN, Ido; MINZEL, Waleed; SNIR-ALKALAY, Irit; VACCA, Joseph; LI, Dansu; (129 pag.)WO2017/21969; (2017); A1;,
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Related Products of 216961-61-4,Some common heterocyclic compound, 216961-61-4, name is tert-Butyl (10-aminodecyl)carbamate, molecular formula is C15H32N2O2, 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 2. Starting compound III: S-Methyl N-cyano-N-(2-methoxy-5-pyridylisothiourea. Starting compound IV: 10-t-Butoxycarbonylaminodecylamine. Purification: Flash chromatography (Eluent 1% NH3(aq) and 0-6% MeOH in CH2Cl2) and crystallization from ether. 13C NMR (CDCl3) delta: 161.2, 158.6, 155.5, 143.3, 137.0, 127.9, 117.3, 110.3, 77.2, 53.2, 41.3, 29.4, 28.9, 28.8, 28.8, 28.6, 28.6, 28.2, 26.2, 26.1

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route tert-Butyl (10-aminodecyl)carbamate, its application will become more common.

Reference:
Patent; Leo Pharmaceutical Products, Ltd. A/S; US6346520; (2002); B1;,
Amide – Wikipedia,
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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 141449-85-6 as follows. category: amides-buliding-blocks

A flask was charged with tert-butyl octahydropyrrolo[3,4-c]pyrrole-2-carboxylate (1.20 g, 5.65 mmol, 1.00 equiv), potassium (bromomethyl)trifluoroboranuide (1.13 g, 5.63 mmol, 1.00 equiv), and THF (15 mL) under nitrogen. The mixture was stirred overnight at 80 C and concentrated under reduced pressure. Potassium carbonate (0.781 g, 5.65 mmol, 1.00 equiv) and acetone (10 mL) were added. The resulting solution was stirred for 2 h at room temperature, dissolved in acetone (2 x 200 mL) and filtered. The filtrate was concentrated under reduced pressure to provide 1.40 g (75% yield) of potassium ((5-(tert- butoxycarbonyl)hexahydropyrrolo[3,4-c]pyrrol-2(lH)-yl)methyl)trifluoroborate as a yellow solid. LCMS (ESI, m/z): 293 [M-K]”.

According to the analysis of related databases, 141449-85-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ABIDE THERAPEUTICS, INC.; GRICE, Cheryl A.; WIENER, John J. M.; WEBER, Olivia D.; DUNCAN, Katharine K.; (364 pag.)WO2018/217805; (2018); A1;,
Amide – Wikipedia,
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Synthetic Route of 14719-21-2, The chemical industry reduces the impact on the environment during synthesis 14719-21-2, name is 2,2,2-Trifluoro-N-(prop-2-yn-1-yl)acetamide, I believe this compound will play a more active role in future production and life.

The mixture of compound 3 (500 mg, 1.18 mmol), Pd (PPh3)4 (145 mg,0.12 mmol, 0.1 eq), CuI (44.5 mg, 0.25 mmol, 0.2 eq), N-(2-propynyl)-2,2,2-trifluoroacetamide (1.07 g,7.08 mmol, 6.0 eq) and triethylamine (0.5 mL, 3.54 mmol, 3.0 eq) in DMF (20 mL) was stirred at roomtemperature overnight. Upon completion of the reaction as monitored by TLC, the mixture wasconcentrated under reduced pressure. The residue was purified by flash chromatography on a silicagel column to provided 310 mg of product 17 as a white solid in 60% yield with an HPLC purity of95%. Rf = 0.40 (dichloromethane-methanol = 10:1). 1H NMR (DMSO-d6, 400 MHz) 10.16 (s, 1H, NH),7.03 (s, 2H, NH2), 5.95 (d, 1H, J = 4.2 Hz, 10-H), 5.36 (d, 1H, J = 6.0 Hz, 20-OH), 5.10 (d, J = 4.2 Hz, 1H,30-OH), 4.74 (t, J = 5.6 Hz, 1H, 50-OH), 4.44-4.55 (m, 1H, 20-H), 4.07-4.17 (m, 1H, 30-H), 3.96 (s, 3H,CH3), 3.76-3.88 (m, 1H, 40-H), 3.37-3.56 (m, 2H, CH2). ESI-MS m/z: 447.1 [M + H]+.

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, 2,2,2-Trifluoro-N-(prop-2-yn-1-yl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ren, Hang; An, Haoyun; Tao, Jingchao; Molecules; vol. 24; 5; (2019);,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 19982-07-1, 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. 19982-07-1, name is N-(3,5-Dimethyladamantan-1-yl)acetamide, This compound has unique chemical properties. The synthetic route is as follows.

l-Acetamido-3,5-dimethyladamantane (44 gm) as obtained in example 1, sodium hydroxide and diethylene glycol are added, and heated to reflux. Then, the contents were maintained for 6 hours at reflux and water (1 175 ml) was added under stirring. The reaction mass was cooled to below 20 C and then added methylene chloride (750 ml), and stirred for 15 minutes at 20C. The layers were separated and the organic layer was distilled off completely under vacuum at below 45C to obtain a residue. The residue was dissolved in ethyl acetate (700 ml). Ethyl acetate hydrochloride (160 ml) was added to the reaction mass and stirred for 5 hours at 25 to 30C. The reaction mass was cooled to 0 to 5C and stirred for 1 hour at 0 to 5 C. The separated solid was filtered and dried at 50C for 2 hours to obtain 87 gm of memantine hydrochloride containing l-amino-3,5,7-trimethyladamantane hydrochloride and l-amino-3-methyladamantane hydrochloride impurity.Memantine hydrochloride: 99.3%;The combined contents of l-amino-3,5,7-trimethyladamantane hydrochloride and 1- amino-3-methyladamantane hydrochloride impurity: 0.5%.

The chemical industry reduces the impact on the environment during synthesis N-(3,5-Dimethyladamantan-1-yl)acetamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; HETERO RESEARCH FOUNDATION; PARTHASARADHI REDDY, Bandi; RATHNAKAR REDDY, Kura; MURALIDHARA REDDY, Dasari; RAJI REDDY, Rapolu; RAMAKRISHNA REDDY, Matta; VAMSI KRISHNA, Bandi; WO2011/125062; (2011); A1;,
Amide – Wikipedia,
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Reference of 108723-79-1, These common heterocyclic compound, 108723-79-1, name is 2-Amino-N,N-diethylacetamide hydrochloride, 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.

To a stirred mixture of 2-amino-N,N-diethylacetamide hydrochloride (64.0 mg, 0.38 mmol) and triethylamine (77.7 mg, 0.77 mmol) in i-PrOH (3 mL) was added 4-chloro-5-[2-methyl-6-(trifluoromethyl)pyridin-4-yl]-6-phenylpyrimidin-2-amine (140.1 mg, 0.38 mmol) at room temperature. After stirring for 16 h at 110 C, the reaction mixture was cooled and concentrated. The residue was purified by Prep-HPLC to afford 2-((2- amino-5-(2-methyl-6-(trifluoromethyl)pyridin-4-yl)-6-phenylpyrimidin-4-yl)amino)-N,N- diethylacetamide (61 mg, 34.6%) as an off-white solid. ES-MS (m/z) [M+l]+ = 459.1.

The synthetic route of 108723-79-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NIKANG THERAPEUTICS, INC.; LOU, Yan; FU, Jiping; HE, Yigang; (0 pag.)WO2020/14332; (2020); A1;,
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Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 174799-52-1, name is tert-Butyl (2-(benzylamino)ethyl)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. category: amides-buliding-blocks

86.63 mg diphenyl cyanocarbonimidate, 52.1 mg isoquinolin-6-amine, and 6 ml THF were added to a reaction bottle with thermal reflux for 3.5 hrs. After removing THF by vacuum, the residue was added to 10 ml EA. The precipitated solid was filtered to obtain 32.9 mg 1-cyano-3-(isoquinolin-6-yl)-2-phenylisourea. The intermediate was reacted with equivalent tert-butyl-2-(benzylamino)ethylcarbamate and 20 mg of DIPEA in 5 ml DMF at 110 C. for 18 hrs. After cooling, 1N NaOH was added and extracted twice with EA. After the combined EA layer was dried and concentrated by Na2SO4, 26.4 mg intermediate product was eluted out by a SiO2 column (EA/Hexane 4:1). The intermediate was added to 1.5 ml 6N HCl at room temperature with stirring overnight. After the reaction solution was evaporated under reduced pressure, 2 ml acetone/methanol (10:1) was added. The precipitate was filtered and washed with acetone, and then the solid was taken and evaporated in vacuum to give 18.7 mg of product.

The synthetic route of tert-Butyl (2-(benzylamino)ethyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Industrial Technology Research Institute; CHEN, Chih-Hung; CHEN, Yi-Hsun; HUANG, Jui-Wen; HUANG, Kuo-Kuei; LIU, Chih-Peng; HWANG, Chrong-Shiong; (22 pag.)US2019/194137; (2019); A1;,
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. 53844-02-3, name is Benzyl (2-bromoethyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 53844-02-3

Step 2 Synthesis of 3-(2-aminoethoxy)benzonitrile hydrobromide: 8 g of benzyl-N-(2-bromoethyl)carbamate, 3.7 g of 3-hydroxybenzonitrile, 4.3 g of calcium carbonate, 5.1 g of potassium iodide and 1.1 g of tetrabutylammonium iodide were stirred in dimethylformamide at 60C. After the treatment with ethyl acetate as the extractant in an ordinary manner, the product was purified by the silica gel column chromatography to obtain 3-[2-(benzyloxycarbonylamino)ethoxy]benzonitrile.

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

Reference:
Patent; Ajinomoto Co., Inc.; EP976722; (2000); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics