Month: September 2021

Related Products of 389890-43-1, 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. 389890-43-1, name is tert-Butyl (cis-3-hydroxycyclobutyl)carbamate, This compound has unique chemical properties. The synthetic route is as follows.

To a mixture of 2,3-dichloro-pyrazine ( 3.0 g, 20 mmol ) and tert-butyl ((1S,3S)- 3-hydroxycyclobutyl)carbamate (see PREPARATION 4A; 3.65 g, 20 mmol) in DMSO (50 mL) was added CS2CO3 ( 13.2 g, 40 mmol), and then the mixture was stirred at 80C overnight. The reaction mixture was diluted with water and filtered. The filter cake was washed with water, and dried to give tert-butyl ((lS,3S)-3-((3-chloropyrazin-2-yl)oxy)cyclobutyl)carbamate (5.7 g, 19.0 mmol, 96.6%). ESI-MS (M+l): 300 calc. for Ci3Hi8ClN303 299.

The chemical industry reduces the impact on the environment during synthesis tert-Butyl (cis-3-hydroxycyclobutyl)carbamate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; AMGEN INC.; ALLEN, Jennifer; FROHN, Michael; HARRINGTON, Paul; PICKRELL, Alexander; RZASA, Robert; SHAM, Kelvin; HU, Essa; WO2011/143366; (2011); A1;,
Amide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 114790-39-5, name is Benzyl (2,2-dimethoxyethyl)carbamate, 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 114790-39-5, Recommanded Product: Benzyl (2,2-dimethoxyethyl)carbamate

Example 1B benzyl allyl(2,2-dimethoxyethyl)carbamate The product of Example 1A (281.0 g, 1.18 mol) in dry toluene (1.0 L) was treated with powdered KOH (291.2 g, 5.20 mol) and triethylbenzylammonium chloride (4.4 g, 0.02 mol). A solution of allyl bromide (188.7 g, 1.56 mol) in toluene (300 mL) was then added dropwise over 1 hour at 20-30 C. The mixture was stirred overnight at room temperature and then water (300 mL) was added over 20 minutes at 20-30 C. The layers were separated and the aqueous phase was extracted with toluene (2*300 mL). The organic phases were combined, washed with brine (2*100 mL), dried (K2CO3), filtered and the filtrate concentrated to provide the title compound. 1H NMR (MeOH-d4, 300 MHz) delta 3.32 (s, 3H) 3.37 (m, 5H), 3.97 (d, J=5.4 Hz, 2H), 4.40-4.50 (m, 1H), 5.15 (m, 4H), 5.75 (m, 1H), 7.23 (m, 5H); MS (DCI/NH3) m/z 297 (M+NH4)+, 280 (M+H)+.

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; Buckley, Michael J.; Ji, Jianguo; US2005/261348; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 98-64-6, These common heterocyclic compound, 98-64-6, name is 4-Chlorobenzenesulfonamide, 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: The prepared TfOH-SiO2 (60 mg, containing 0.05 mmol TfOH) was added to the toluene (2 mL) solution of alkene (2 mmol or 4 mmol) and sulfonamide (1 mmol) and the reaction mixture was stirred at 70 oC (or 85 oC). The course of the reaction was monitored by TLC. After the completion of the reaction, the mixture was cooled to room temperature and the reactor was centrifuged (2000 r/min) for 2 min and the solution was removed by syringe. The catalyst was then washed with toluene (1 mL) twice with the same procedure and a new reaction was carried out by adding the new batch of alkene (2 mmol), sulfonamide (1 mmol) and toluene (2 mL) to the recovered catalyst. The solution containing the product was purified through a silica gel flash column to afford the product.

The synthetic route of 98-64-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Pei Nian; Xia, Fei; Zhao, Zheng Le; Wang, Qing Wei; Ren, Yu Jie; Tetrahedron Letters; vol. 52; 46; (2011); p. 6113 – 6117;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 25900-61-2, name is 3-Amino-N-methylbenzamide, 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 25900-61-2, Recommanded Product: 3-Amino-N-methylbenzamide

Step 4 Synthesis of 3-{2-[4-(5-Fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-2-oxo-acetylamino}-N-methyl-benzamide [4-(5-Fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-oxo-acetyl chloride (105 mg, 0.286 mmol) (prepared by the similar method described in example 57, Step-2 using 5-Fluoro-2-trifluoromethyl-phenyl)-piperazin-1-yl-methanone hydrochloride salt as starting material which is being prepared by the general method mentioned in the earlier examples using 5-fluoro-2-trifluoromethyl benzoic acid as starting material, Aldrich, St. Louis, Mo.) in DCM (2.5 mL) was added to cold(0 C.) solution of 3-Amino-N-methyl-benzamide (43 mg, 0.28 mmol), Et3N (86 mg, 0.12 mL, 0.86 mmol) in DCM (2.5 mL) and stirring was continued at ambient temperature for 2 hr. The reaction mixture was diluted with DCM, washed with cold water, followed by 2N HCl and brine solution. The organic layer thus collected was dried over sodium sulphate, concentrated under reduced pressure to afford the residue. The residue obtained was purified by recrystallisation from a mixture of ethyl acetate and hexane to afford 70 mg (51.09%) of 3-{2-[4-(5-Fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-2-oxo-acetylamino}-N-methyl-benzamide. LCMS Purity: 99.7%. 1H NMR (DMSO-d6): delta 10.95 (d, 1H), 8.4 (m, 1H), 8.2-8.0 (d, 1H), 8.6-7.9 (m, 1H), 7.8-7.6 (m, 1H), 7.6-7.4 (m, 4H), 3.9-3.4 (m, 6H), 3.3-3.1 (m, 2H), 2.8 (m, 3H).

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; Bischoff, Alexander; Subramanya, Hosahalli; Sundaresan, Kumar; Sammeta, Srinivasa Raju; Vaka, Anil Kumar; US2010/160323; (2010); 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. 116332-54-8, name is 4-Fluoro-N-methoxy-N-methylbenzamide, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 4-Fluoro-N-methoxy-N-methylbenzamide

(b) 4-Fluoro-2-(4-pyridyl)acetophenone–A solution of lithium diisopropylamide was prepared at -78 C. in the usual manner from diisopropylamine (21 ml, 0.15 mol) and n-bultyllithium (54 mL of 2.5M solution in hexanes, 0.135 mol), and to this was added at -78 C., 4-picoline (10 g, 0.108 mol). After Stirring an additional 15 min at -78 C., 4-fluoro-N-methoxy-N-methylbenzamide (20 g, 0.109 mol) was added, and the mixture was allowed to slowly warm to rt. The reaction mixture was poured into saturated aqueous NaCl and extracted with 4:1 THF/CH2 Cl2, and the organic extract was dried (MgSO4). The solvent was removed in vacuo, and to the oily brown residue was added Et2 O. The title compound was obtained as a brown solid (16.8 g, 72%) which was recrystallized from Et2 O/Hex: 1 H NMR (CDCl3): d 8.55 (d, 2H); 8.03 (dd, 2H); 7.16 (m, 4H); 4.24 (s, 2H).

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 116332-54-8.

Reference:
Patent; SmithKline Beecham Corporation; US5916891; (1999); A;,
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. 193751-54-1, name is tert-Butyl cyclopent-3-en-1-ylcarbamate, A new synthetic method of this compound is introduced below., Recommanded Product: tert-Butyl cyclopent-3-en-1-ylcarbamate

product was obtained which was recrystallised twice from heptane. After crystallization, 1.01 g of syn epoxide was obtained in the form of white needles. The mother liquors were subjected to chromatography (silica, toluene/EtOAc = 9:1 – 7:1) to yield 3.51 g of anti epoxide in the form of a white amorphous solid. [0058] Syn epoxide: is NMR (400MHz, DMSO-d6, delta, ppm, characteristic signals): 1.36 (s, 9H), 6.79 (d, 1H, J=8Hz), 1.47 (dd, 1H, J=8Hz and 14Hz), 2.17 (dd, 1H, J=8Hz and 14Hz), 3.44 (s, 2H), 3.54 (m, 1H). MS-ESI+ (m/z): 200 (M + H). TLC: toluene/EtOAc = 3:1, Rf = 0.4. [0059] Anti epoxide: 1H NMR (400MHz, DMSO-d6, delta, ppm, characteristic signals): 1.35 (s, 9H), 1.78 (d, 2H, J=15Hz), 1.98 (dd, 1H, J=8Hz and 15Hz), 3.51 (s, 2H), 3.89 (q, 1H, J=8 and 16Hz), 5.70 (d, 1H, J=8Hz). MS-ESI+ (m/z): 200 (M + H). TLC: toluene/EtOAc = 3:1, Rf = 0.45.

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; Nabriva Therapeutics AG; Mang, Rosemarie; Thirring, Klaus; Heilmayer, Werner; EP2433926; (2012); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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 123986-64-1 as follows. Quality Control of tert-Butyl 4-(hydroxymethyl)benzylcarbamate

The compound (18.0 g) obtained in Example 103-2 was dissolved in chloroform (540 ml) and then added with manganese dioxide (chemically processed product) (118 g), followed by stirring at room temperature for 15 hours. The reaction solution was filtrated through Celite and the filtrate was then concentrated under reduced pressure. The residue was purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (17.1 g) as a white solid.

According to the analysis of related databases, 123986-64-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Kureha Chemical Industry Co., Ltd.; EP1550657; (2005); 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. 39549-79-6, name is 2-Amino-4-methylbenzamide, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 39549-79-6

2-amino-4-methylbenzamide (4.93 g, 32.8 mmol) obtained in above was added with formic acid (30 mL, 787.9 mmol), followed by stirring for 6 hours at 100° C. The reaction mixture was cooled to room temperature, concentrated under reduced pressure, and washed with water. The filtered solid was dried with warm wind in an oven (40° C.) for 6 hours or more to obtain the title compound (4.79 g, 91percent). 1H-NMR Spectrum (300 MHz, DMSO-d6): delta 8.06 (s, 1H), 8.00 (d, 1H), 7.47 (s, 1H), 7.34 (d, 1H), 2.45 (s, 3H) MS (ESI+, m/z): 161 [M+H]+

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 39549-79-6.

Reference:
Patent; HANMI PHARM. CO., LTD; Bae, In Hwan; Son, Jung Beom; Han, Sang Mi; Kwak, Eun Joo; Kim, Ho Seok; Song, Ji Young; Byun, Eun Young; Jun, Seung Ah; Ahn, Young Gil; Suh, Kwee Hyun; US2014/371219; (2014); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 75175-77-8, name is 3-(4-Fluorophenyl)-N,N-dimethylacrylamide, molecular formula is C11H12FNO, 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. Quality Control of 3-(4-Fluorophenyl)-N,N-dimethylacrylamide

General procedure: Cyanothioacetamide (for X=S) (1.5 equiv) or cyanoacetamide (for X=O) (1.5 equiv) was added to a solution of the 1, 3-diones (for R4= -CF3 and -CH3) (1.0 equiv) or enaminones (for R4=H) (1.0 equiv) in ethanol in the presence of DABCO (1.0 equiv) at room temperature. The reaction mixture was stirred under reux for 3-6 h until complete conversion of the starting materials, as monitored by TLC. After cooled to room temperature, the solvent was evaporated under reduced pressure and the residue was neutralized with diluted hydrochloric acid (1 N) to precipitate the crude products. After filtrated and dried in vacuo, the product can be straight used for step d. Yield: 70-90%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 75175-77-8, its application will become more common.

Reference:
Article; Wang, Ning-Yu; Zuo, Wei-Qiong; Xu, Ying; Gao, Chao; Zeng, Xiu-Xiu; Zhang, Li-Dan; You, Xin-Yu; Peng, Cui-Ting; Shen, Yang; Yang, Sheng-Yong; Wei, Yu-Quan; Yu, Luo-Ting; Bioorganic and Medicinal Chemistry Letters; vol. 24; 6; (2014); p. 1581 – 1588;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 94838-59-2, These common heterocyclic compound, 94838-59-2, name is tert-Butyl 4-aminophenethylcarbamate, 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 15 – Preparation of tert-Butyl (4-(2-chloroacetamido)phenethyl)carbamate. tert-Butyl (4-aminophenethyl)carbamate prepared according to Example 14 (7.50 grams, 31.7 mmol, 1.0 eq) was dissolved in CH2C12 (500 mL) and cooled to 0C in an ice bath. DMAP (6.23 g, 51.0 mmol, 1.6 eq) was added in one go and the mixture was allowed to stand for 10 minutes before a solution of chloroacetyl chloride (3.00 ml, 37.7 mmol, 1.2 eq) in 100 ml CH2C12 was added drop wise over 20 minutes to the stirring mixture. The mixture was then left at 0C for 30 minutes and at room temperature for 3 hours before it was concentrated under reduced pressure. The sticky red residue was dissolved in CH2C12 (250 mL) and washed with 0.5 M aqueous acetic acid (2 x 200 mL), 0.5 M aqueous NaHC03 (1 x 100 mL) and dried on anhydrous K2C03. The solution was filtered through a (4 cm x 5 cm long) silica gel plug using 75% ethyl acetate in heptane to elute. Removal of the volatiles under reduce pressure yielded 7.46 g of the title compound (23.8 mmol, 75%). 1H NMR (300 MHz, DMSO- ) 6 10.21 (s, 1H), 7.49 (d, J= 8.4 Hz, 2H), 7.14 (d, J= 8.4 Hz, 2H), 6.84 (t, J= 5.6 Hz, 1H), 4.23 (s, 2H), 3.18 – 2.99 (m, 2H), 2.74 – 2.56 (m, 2H), 1.36 (s, 9H). 13C NMR (101 MHz, DMSO) delta 164.4, 155.5, 136.5, 134.9, 128.9, 119.4, 77.4, 43.5, 41.5, 34.9, 28.2.

Statistics shows that tert-Butyl 4-aminophenethylcarbamate is playing an increasingly important role. we look forward to future research findings about 94838-59-2.

Reference:
Patent; UNIVERSITETET I OSLO; GOLDING, Louise; RONGVED, Pal; ASTRAND, Ove Alexander H°gmoen; BAYER, Annette; LEIROS, Hanna-Kirsti Schr°der; SAMUELSEN, Ørjan; EDVARDSEN, Kine Susann Waade; WO2015/49546; (2015); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics