Month: September 2021

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. 227940-71-8, name is tert-Butyl 7-benzyl-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 227940-71-8

7-Benzyl-3,7-diazabicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (0.49 g, 1.6 mmol) was dissolved in methanol (20 ml.) and 20% Pd(OH)2/C (wet) (~ 2 g) was added under a nitrogen atmosphere. This mixture was warmed to about 50 0C and shaken for 2 h under 55 psi of hydrogen. The resulting mixture was filtered and concentrated to give 0.32 g (94% yield) of the title compound (MS m/z 227 (M+H)).

The synthetic route of 227940-71-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TARGACEPT, INC.; WO2009/111550; (2009); A1;,
Amide – Wikipedia,
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. Formula: C14H22N2O2

Tert-butyl(2-(benzylamino)ethyl)carbamate (Formula II, 50 g, 0.200 moles), 1,8-Diazabicycloundec-7-ene (61.12 ml, 0.401 moles) and DMF (300 ml) were charged in round bottom flask at RT and stirred to get heterogeneous solution. The reaction mixture was cooled to 0-5 C. and methyl vinyl ketone (75.3 ml, 0.903 moles) was added to the reaction mixture slowly over a period of 30 min. The resulting reaction mixture was stirred at room temperature for 16 h. After completion of the reaction, the reaction mixture was cooled to 0-5 C. and diluted with water (500 ml). The aqueous solution was extracted with ethyl acetate (250 ml*2). The organic layer was washed with 1N HCL (200 ml). The pH of aqueous layer was adjusted to 8 with saturated NaHCO3 solution (200 ml) and extracted with ethyl acetate (250 ml*2). The combined organic layers were dried over sodium sulfate, filtered and concentrated under reduced pressure at 45-50 C. to give tert-butyl(2-(benzyl(3-oxobutyl)amino)ethyl)carbamate (Formula III, 30 g, yield 46.87%) as a dark brown color liquid.

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

Reference:
Patent; DR. REDDY’S LABORATORIES LIMTED; IQBAL, Javed; DAHANUKAR, Vilas Hareshwar; ORUGANTI, Srinivas; KANDAGATLA, Bhaskar; (23 pag.)US2016/168138; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 17193-28-1, A common heterocyclic compound, 17193-28-1, name is 1-Amino-1-cyclopentanecarboxamide, molecular formula is C6H12N2O, 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.

1 -Fluoropentanoic acid (22, 350 mg, 2.91 mmol) were dissolved in dry dimethylfor- mamide (= DMF) (5 ml_) and triethylamine (= Et3N) (486 mI_, 353 mg, 3.49 mmol) was added. Then 1 -aminocyclopentanecaroxamide (373 mg, 2.91 mmol) and (2- (1 FI-benzotriazol-1 -yl)-1 ,1 ,3,3-tetramethyluronium hexafluorophosphate) (= FIBTU) (1324 mg, 3.49 mmol) were added. The mixture was stirred for 24 h at room tem- perature (= r.t.). Then water was added and the mixture was extracted wit ethyl ac- etate (3x). The combined organic layer was washed with water, saturated NaFIC03 solution and brine (2x), dried over Na2S04, filtered and evaporated to dryness in vacuo. The residue was purified by flash column chromatography (dichloro- methane/methanol = 98/2; Rf = 0.2) to yield 23 (668 mg, 99%) as colorless solid.1H NMR (400 MHz, CDCIs): d = 4.76 (t, J = 5.7 Hz, 1 H), 4.61 (t, J = 5.7 Hz, 1 H), 2.43 – 2.34 (m, 2H), 2.30 – 2.22 (m, 2H), 2.07 – 1 .99 (m, 2H), 1 .94 – 1 .73 (m, 8H) ppm.13C NMR (101 MHz, CDCIs): d = 175.57, 170.07, 82.94, 69.19, 34.94, 34.64,29.77, 29.62, 23.00, 21 .95 ppm.MS: 231 .05 [M+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; JULIUS-MAXIMILIANS-UNIVERSITAET WUERZBURG; CHEN, Xinyu; DECKER, Michael; HIGUCHI, Takahiro; HOFFMANN, Matthias; (0 pag.)WO2019/134765; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 121492-06-6, name is N-Boc-(2-Aminoethyl)-N-methylamine, 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 121492-06-6, COA of Formula: C8H18N2O2

To a cooled (-5 C) solution of Lambda/-(2-aminoethyl)-Lambda/-methylcarbamic acid-te/-butyl ester (5 g , 28.7 mmol) in ethanol (60 ml) was added triethylamine. 2-Chloro-4,6-dimethoxy-5-nitropyrimidine (Intermediate 13; 4 g, 18.2 mmol) was added portion-wise over a period of ca. 10 min. The mixture was stirred for a further hour at 0 0C (reaction complete according to analysis (TLC). The ethanol was then removed under reduced pressure and the resulting yellow oil was purified by column chromatography (SiO2, 1 :2 ethyl acetate: petroleum ether) to give a yellow solid (3.76 g; 58%). m/z 358.21 (MH+).

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; PARADIGM THERAPEUTICS LTD.; WO2007/582; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 22246-76-0, These common heterocyclic compound, 22246-76-0, name is 8-Amino-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one, 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.

Example No. 217Preparation of methyl 3- (7- ( (2-oxo-2 , 3 , 4 , 5-tetrahydro-lH- benzo [b] azepin-8-yl) amino) -IH-pyrazolo [4, 3-d] pyrimidin- 5- yl) benzoate methyl 3- (7-chloro-2- (4-methoxybenzyl) -2H-pyrazolo [4,3- d] pyrimidin- 5 -yl) benzoate (0.16 mmol) and 8 -amino-4 , 5 -dihydro- lH-benzo [b] azepin-2 (3H) -one (0.3 mmol 2 eq. , ) were suspended in MeOH (dry, 3mL) in a microwave vial (2-5mL) , HC1 in dioxane (4M, 3 drops) was added. The reaction mixture was irradiated in a microwave reactor for 5 min at 140C. The reaction mixture was evaporated and used without further purification. The residue was dissolved in TFA (3mL) . The reaction mixture was irradiated in a microwave reactor for 5 min at 140C. The reaction mixture was concentrated and purified by semi- preparative HPLC-MS and freeze dried from water/t-BuOH 4/1. exact mass: 428.1868 g/molHPLC-MS: analytical method Lrt: 4.65 min – found mass: 429 (m/z+H)

The synthetic route of 22246-76-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ORIGENIS GMBH; ALMSTETTER, Michael; THORMANN, Michael; TREML, Andreas; TRAUBE, Nadine; WO2012/143144; (2012); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 2297-06-5, name is Methyl 4-amino-2-sulfamoylbenzoate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H10N2O4S

SYNTHESIS EXAMPLE 5 Synthesis of preparation intermediate, methyl 2-(aminosulfonyl)-4-(2,5-dihydro-3,4-dimethyl-2,5-dioxo-1H-pyrrol-1-yl)benzoate (Compound No. II-B-4) In 3 ml of acetic acid, 1 mmol of methyl 4-amino-2-(aminosulfonyl)benzoate and 1.05 mmol of 2,3-dimethylmaleic anhydride were stirred at 80 C. for 40 hours. Acetic acid was then distilled off from the reaction mixture, followed by the addition of 20 ml of ice water to the oily residue. After the mixture thus formed was stirred for 2 hours, the resulting precipitate was collected by filtration and then dried in air. Yield: 43%. Its physiocochemical properties are shown in Table 8.

The synthetic route of 2297-06-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kureha Kagaku Kogyo K.K.; US5127937; (1992); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 13304-62-6, 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. 13304-62-6, name is N-Benzylacrylamide, This compound has unique chemical properties. The synthetic route is as follows.

The preparation method is as follows: Add a N-benzyl acrylamide dioxane solution to a clean 30 mL round bottom flask with stirring magnets at a concentration of 1 M. Then adding the catalyst cerium acetate (10 mol%), Oxidant silver carbonate (3 eq), additive potassium hexafluorophosphate (0.5 eq), 1,2-diphenylacetylene (1.0 eq). This mixture was stirred at room temperature for one hour and then heated to reflux overnight. The reaction was detected by thin plate chromatography, and after the reaction was completed, it was cooled to room temperature, and the reaction was quenched with water. Extract 4×20 mL with ethyl acetate and wash with saturated brine. Dry over anhydrous sodium sulfate and remove sodium sulfate by filtration. The solvent was evaporated under reduced pressure to give a crude material. Using petroleum ether/ethyl acetate as the eluent, Purified by column chromatography (mobile phase: ethyl acetate / petroleum ether = 1/2) A pale yellow solid product was obtained in a yield of 60%.

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

Reference:
Patent; Lanzhou University; Li Yumin; Chen Hao; Han Zhijian; (27 pag.)CN109928969; (2019); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 830-43-3, These common heterocyclic compound, 830-43-3, name is 4-(Trifluoromethyl)benzenesulfonamide, 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.

In the same manner as in Example 158, 0.390 g of 1-(2-chlorobenzyl)-2-methyl-6-[4-(trifluoromethyl)benzenesulfonylcarbamoyl]benzimidazole (221) were formed from 0.45 g of 6-carboxy-1-(2-chlorobenzyl)-2-methylbenzimidazole, 0.486 g of N,N’-carbonyldiimidazole, 0.676 g of 4-(trifluoromethyl)benzenesulfonamide and 0.457 g of diazabicycloundecene. Properties of Compound (221): 1H-NMR(DMSO-d6, delta): 2.52(3H, s), 5.62(2H, s), 6.47(1H, d, J=7.2 Hz), 7.22(1H, t, J=7.5 Hz), 7.34(1H, t), 7.56(1H, d, H=8.0 Hz), 7.66(1H, d, 8.5 Hz), 7.78(1H, d), 7.97(2H, d, J=8.3 Hz), 8.06(1H, s), 8.15(2H, d, J=8.3 Hz). IR(KBr): 1620 cm-1. Mass(FAB): m/e 508(M+1). mp: 288.0-292.0 C.

Statistics shows that 4-(Trifluoromethyl)benzenesulfonamide is playing an increasingly important role. we look forward to future research findings about 830-43-3.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US6352985; (2002); B1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 2618-96-4, These common heterocyclic compound, 2618-96-4, name is Dibenzenesulfonimide, 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.

General procedure: Under N2, ynamide 1a (0.300 mmol, 108.7 mg) and diphenylsulfonimide (2a; 0.600 mmol, 178.4 mg, 2.00 equiv) were dissolved in CH2Cl2 (4.00 mL). The reaction mixture was allowed to stir at r.t. After the consumption of 1a (4.5 h, TLC, eluent: PE-EtOAc, 4:1), the mixture was concentrated, and the residue was purified by flash chromatography on silica gel (eluent: PE-EtOAc, 6:1 ? 4:1) to afford 3a.

The synthetic route of 2618-96-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yu, Lian; Deng, Yuan; Cao, Jian; Synthesis; vol. 47; 6; (2015); p. 783 – 788;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 956434-30-3, name is tert-Butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C13H17ClN2O3

(step 1) To a solution of (2R)-3-methylbutan-2-ol (0.38 mL) in toluene (8 mL) was added sodium hydride (0.28 g), and the resulting mixture was stirred at 70C for 15 min under a nitrogen atmosphere. A mixture of tert-butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (1.0 g), BINAP (0.066 g), Pd2(dba)3 (0.048 g) and toluene (8 mL) was added, and the resulting mixture was stirred at 100C for 2 hr under an argon atmosphere. The reaction solution was poured into water, and the resulting product was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (solvent gradient; 0?40% ethyl acetate/hexane) to give tert-butyl 8-{[(1R)-1,2-dimethylpropyl]oxy}-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (0.77 g, 65%) as a white powder. 1H-NMR(CDCl3):delta0.94(3H,d,J=6.8Hz), 0.96(3H,d,J=6.6Hz), 1.23(3H,d,J=6.2Hz), 1.43(9H,s), 1.82-1.95(1H,m), 3.81(2H,brs), 4.21(2H,brs), 4.34-4.43(2H,m), 4.97(1H,brs), 6.40(1H,brs), 7.30-7.50(1H,m)

According to the analysis of related databases, 956434-30-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP2213675; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics