Tag: M.W=100-200

Related Products of 75175-77-8, 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 75175-77-8 as follows.

General procedure: In a 50 ml round-bottom flask, substituted enaminones (1 mmol), hydrazine hydrate (1.3 mmol) or phenyl hydrazine (1 mmol) and [crown ether MIm][HSO4] (20 mol%) were charged. The reaction mixture was stirred at 50 C under solvent-free conditions for 10-35 min. After completion of reaction (monitoredby TLC), the reaction mixture was extracted with ethyl acetate (2 9 10 ml). The extracted ethyl acetate was evaporated in a rotary evaporator and the desired product was isolated from the resultant mass by column chromatography (petether: ethyl acetate, 9.5: 0.5). Finally, the catalyst was recycled and used for thenext run.

According to the analysis of related databases, 75175-77-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Patil, Dayanand; Chandam, Dattatraya; Mulik, Abhijeet; Jagdale, Suryabala; Patil, Prasad; Deshmukh, Madhukar; Research on Chemical Intermediates; vol. 41; 9; (2015); p. 6843 – 6858;,
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. 188345-71-3, name is 2-Boc-2-Azabicyclo[2.2.1]hept-5-ene, A new synthetic method of this compound is introduced below., SDS of cas: 188345-71-3

2-(Tert-butoxycarbonyl)-2-azabicyclo[2.2.1]hept-5-ene was dissolved in 200 mL of dichloromethane-methanol (2:1), and the solution was cooled to -78 C. Ozone was passed through the solution until it turned blue and then for a further 10 min. Argon was bubbled through the solution to remove excess ozone (the solution turned colorless). This process (ozone, followed by argon) was repeated one more time to ensure complete formation of the ozonide. Sodium borohydride (3.7 g, 97 mmol) was carefully added to the reaction mixture at -78 C., and the resulting mixture stirred for 16 h, as the temperature of the reaction was gradually increased to ambient. Saturated ammonium chloride solution (100 mL) was added, and the mixture was stirred for an additional 1 h. The mixture was extracted with dichloromethane (2¡Á150 mL), and the combined organic extracts were dried over anhydrous magnesium sulfate. The solvent was removed by rotary evaporation to give 1-(tert-butoxycarbonyl)-2,4-bis(hydroxymethyl)pyrrolidine, as a light yellow oil.

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; Targacept, Inc.; US2011/263629; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 96-30-0, 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 96-30-0 as follows.

In a sealed tube, intermediate 77 (287.19 mg, 2.67 mmol) was added to a solution of 6-chloro-4-nitroindole (350.00 mg, 1.78 mmol) and Cs2CO3 (870.11 mg, 2.67 mmol) in dryDMF (3.5 mL) under N2. The mixture was stirred at 90 C for 17 h. The reaction mixturewas diluted with EtOAc and water and the layers were separated. The organic layer waswashed with brine, dried over MgSO4 and filtered. The solvent was removed under reduced pressure to give 378 mg of intermediate 67 (79% yield, brown solid) which was directly engaged in the next step without further purification.

According to the analysis of related databases, 96-30-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; STANSFIELD, Ian; QUEROLLE, Olivier, Alexis, Georges; LIGNY, Yannick, Aime, Eddy; GROSS, Gerhard, Max; JACOBY, Edgar; MEERPOEL, Lieven; GREEN, Simon, Richard; HYND, George; KULAGOWSKI, Janusz, Jozef; MACLEOD, Calum; MANN, Samuel, Edward; (419 pag.)WO2018/2219; (2018); A1;,
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. 1746-77-6, name is Isopropyl carbamate, This compound has unique chemical properties. The synthetic route is as follows., category: amides-buliding-blocks

EXAMPLE 113 4-[[[3-[(aminoiminomethyl)amino]phenyl]carbonyl]amino]-2-methoxy-N-[(1-methylethoxy)carbonyl]phenylalanine, trifluoroacetate salt, monohydrate STR330 Steps A/B/C STR331 The above compound was prepared from methyl pyruvate, isopropylcarbamate and 2-bromo-5-nitro anisole using the procedures described in Example 76 Steps A, B and C.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1746-77-6.

Reference:
Patent; G. D. Searle & Co.; US5952381; (1999); A;,
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. 2835-68-9, name is 4-Aminobenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C7H8N2O

General procedure: To a 25 mL Schlenk tube containing a solution of 2 in 2 mL of THF was added amide (1.0 mmol) and (EtO)3SiH (0.50 g, 3.0 mmol). The reaction mixture was stirred at 60 C until there was no amide left (monitored by TLC and GC-MS). The product was purified according to literature procedures by Beller

The synthetic route of 2835-68-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ren, Shishuai; Wang, Yangyang; Yang, Fei; Sun, Hongjian; Li, Xiaoyan; Catalysis Communications; vol. 120; (2019); p. 72 – 75;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 758-96-3, name is N,N-Dimethylpropionamide, molecular formula is C5H11NO, 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. SDS of cas: 758-96-3

4-Methoxy-7-propionyl-2-trifluoromethyl-1H-benzimidazole The compound of Example 105 (800 mg) was dissolved in THF (20.0 mL) under an argon gas atmosphere, and a 1.58 mol/L n-butyl lithium/hexane solution (3.90 mL) was added dropwise thereto at -78C, followed by stirring for 1 hour as it was. Thereafter, N,N-dimethyl propionamide (0.890 mL) was added thereto at the same temperature, followed by stirring for 3 hours while warming to room temperature. To the reaction liquid was added a saturated aqueous ammonium chloride solution, followed by extraction with ethyl acetate. The organic layer was washed with water and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was then purified by silica gel column chromatography (chloroform) to obtain the desired product (342 mg) as a white powder. EIMS (+): 272 [M]+. 1H NMR (CDCl3, 400 MHz): delta 1.29 (3H, t, J=7.3 Hz), 3.08 (2H, q, J=7.3 Hz), 4.15 (3H, s), 6.80 (1H, d, J=8.6 Hz), 7.96 (1H, d, J=8.6 Hz), 11.4 (1H, brs).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 758-96-3, its application will become more common.

Reference:
Patent; Kyorin Pharmaceutical Co., Ltd.; EP2168959; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 20188-40-3,Some common heterocyclic compound, 20188-40-3, name is 4-(Aminomethyl)benzamide hydrochloride, molecular formula is C8H11ClN2O, 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.

Ethyl 2-(2-fluoro-4-propylphenoxy)-4-formylnicotinate (0.13 g) obtained in Reference Example 319 was dissolved in methanol (3 mL), 4-(aminomethyl)benzamide hydrochloride (0.082 g), acetic acid (0.024 g) and triethylamine (0.061 g) were added, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added sodium tetrahydroborate (0.15 g), and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with water and ethyl acetate. The organic layer was separated, washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by NH silica gel chromatography (hexane-ethyl acetate), and recrystallized from ethyl acetate-ethanol to give the title compound (0.079 g). MS: [M+H]+ 420.2 1H NMR (300 MHz, DMSO-d6) delta0.93 (3H, t, J = 7.3 Hz), 1.63 (2H, sxt, J = 7.4 Hz), 2.56-2.65 (2H, m), 4.48 (2H, s), 4.76 (2H, s), 7.02-7.14 (1H, m), 7.16-7.28 (2H, m), 7.34 (2H, d, J = 5.1 Hz), 7.38 (2H, d, J = 8.3 Hz), 7.87 (2H, d, J = 8.3 Hz), 7.94 (1H, brs), 8.20 (1H, d, J = 5.1 Hz).

The synthetic route of 20188-40-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Pharmaceutical Company Limited; SUGIMOTO, Takahiro; NAKAMURA, Minoru; SAKAMOTO, Hiroki; SUZUKI, Shinkichi; YAMADA, Masami; KAMATA, Makoto; KOJIMA, Takuto; FUJIMORI, Ikuo; SHIMOKAWA, Kenichiro; EP2921480; (2015); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 154350-29-5, These common heterocyclic compound, 154350-29-5, name is Cyclopropanesulfonamide, 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 an iced slurry of cyclopropanesulfonamide (1.21 g, 9.99 mmol), Triethylamine (2.95 mL, 20.97 mmol), and 4-Dimethylaminopyridine (0.061 g, 0.499 mmol) in CH2Cl2 (50 mL) was added solution of Di-tert-butyl dicarbonate (2.423 mL, 10.99 mmol) in DCM (10 mL) dropwise. The formed solution was stirred at room temperature overnight, Removed the solvent in vacuo. The residual oil was taken up in EtOAc and washed with 1M HCl and brine. Dried over MgSO4, filtered, and concentrated. The residue was purified by Biotage column, eluted with gradient 5percent50percent acetone-hexane to yield the desired produce tert-butyl cyclopropylsulfonylcarbamate (2.17 g, 9.61 mmol, 96percent yield) as a viscous oil, which solidified upon standing on bench. 1H NMR (400 MHz, CDCl3) ppm 1.11-1.13 (m, 2H) 1.37-1.39 9m, 2H) 1.53 (s, 9H), 2.89-2.92 (m, 1H) 7.00-7.05 (b, NH).

The synthetic route of 154350-29-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2010/150866; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 3984-14-3, These common heterocyclic compound, 3984-14-3, name is N,N-Dimethylsulfamide, 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 5 (+/-)8-cyclohexyl-N-[(dimethylamino)sulfonyl]-1,1a,2,12b-tetrahydro-1a-(4-morpholinylcarbonyl)-cycloprop[d]indolo[2,1-a][2]benzazepine-5-carboxamide. A 2M solution of oxalyl chloride (0.093 mL, 0.186 mmol) in CH2Cl2 was added dropwise to a solution of (+/-)-8-cyclohexyl-1,1a,2,12b-tetrahydro-1a-(4-morpholinylcarbonyl)-cycloprop[d]indolo[2,1-a][2]benzazepine-5-carboxylic acid (45 mg, 0.093 mmol) in CH2Cl2 (10 mL), containing one drop of DMF. The reaction mixture was stirred at rt. for 2 hr., after which it was concentrated and dried under high vacuum. The residue was subsequently dissolved in THF (10 mL) and a solution of N,N-dimethylsulfonamide, (23 mg, 0.186 mmol) and DIPEA (0.049 mL, 0.279 mmol)) in THF (2 mL) was added. This was followed by the addition of DMAP (10 mg), after which the reaction was stirred at rt. for 10 min., and then at 50 C. overnight. It was then cooled, and the mixture concentrated under reduced pressure. The resultant residue was purified by preparative reverse phase HPLC to afford the product as a yellow solid, (5.0 mg, 9% yield). MS m/z 591(MH+), Retention time: 3.525 min; 1H NMR (300 MHz, CD3OD) delta ppm. Compound was observed to exist as inter-converting rotamers, as evidenced from the compound’s NMR spectrum.

The synthetic route of 3984-14-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/60565; (2007); 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. 5202-85-7, name is 2-Amino-5-chlorobenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C7H7ClN2O

General procedure: To an oven-dried 20 cm3 test tube with a ground-in stopperequipped with a stir bar were added anthranilamide (1.0 mmol), benzyl alcohol (1.0 mmol), KOH (2.0 mmol),and 4 cm3 toluene. The test tube was put in an oil bath potpreheated at 90 C and the mixture was stirred for 20 h at90 C. After cooling to room temperature, the reactionmixture was added about 5 g silica gel and directly condensedon a rotator under vacuum. The resulting residualwas transferred to a silica gel chromatography column andeluted with a solution of petroleum ether and ethyl acetate[4/1 (v/v)] to give a white solid 2-phenyl-4(3H)-quinazolinone.For some products (3f, 3g, 3n, and 3t) onlysparingly soluble in ethyl acetate, the reaction mixtureswere condensed in vacuo on a rotary evaporator. Theresiduals were washed three times with water and oncewith ethyl acetate, and then dried in an infrared oven togive the desired products pure enough for NMR analysis.

The synthetic route of 5202-85-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qiu, Dezhi; Wang, Yanyan; Lu, Dongming; Zhou, Lihong; Zeng, Qingle; Monatshefte fur Chemie; vol. 146; 8; (2015); p. 1343 – 1347;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics