scholarly journals An Efficient Synthesis of Milnacipran Hydrochloride via Reductive Amination of Aldehyde

2017 ◽  
Vol 2017 ◽  
pp. 1-6
Author(s):  
Neha Reddy Desireddy ◽  
Arava Glory ◽  
Krishna Reddy Bhimireddy ◽  
Yadagiri Kurra ◽  
Ram Reddy
Keyword(s):  
Primary Amine ◽  
Reductive Amination ◽  
Major Product ◽  
Important Application ◽  
Water Soluble ◽  
High Yield ◽  
Efficient Synthesis ◽  
By Products

An efficient synthesis of milnacipran hydrochloride has been accomplished. The important application of this paper is the reductive amination of aldehyde to primary amine with water soluble reagents. This method provides a high yield of primary amine as the major product, reduces the number of steps, and discourages by-products.

Bromination of Tetralin. Short and Efficient Synthesis of 1,4-Dibromonaphthalene

2000 ◽  
Vol 65 (11) ◽  
pp. 1791-1804 ◽  
Author(s):  
Osman Çakmak ◽  
Ismail Kahveci ◽  
Íbrahim Demirtaş ◽  
Tuncer Hökelek ◽  
Keith Smith
Keyword(s):  
High Temperature ◽  
Major Product ◽  
High Yield ◽  
Efficient Synthesis ◽  
Secondary Products ◽  
Derivatives Of ◽  
Sole Product

High-temperature bromination of tetralin (1,2,3,4-tetrahydronaphthalene) with bromine resulted in benzylic bromination to give 1,4-dibromo-1,2,3,4-tetrahydronaphthalene (4) as a major product and several secondary products. Photolytic bromination of tetralin and subsequent double dehydrobromination of 1,1,4,4-tetrabromo-1,2,3,4-tetrahydronaphthalene (10) gave 1,4-dibromonaphthalene (11) as the sole product in a high yield. 1,4-Dibromonaphthalene is efficiently converted to the corresponding methoxy (12 and 13) and cyano (14 and 15) derivatives of naphthalene.

scholarly journals Full N,N-Methylation of 4,4′-Methylenedianiline with Dimethyl Carbonate: A Feasible Access to 4,4′-Methylene bis(N,N-Dimethylaniline)

2018 ◽  
Vol 2018 ◽  
pp. 1-10
Author(s):  
Zegang Qiu ◽  
Kunjie Wang ◽  
Zhiqin Li ◽  
Tao Li ◽  
Jinhao Bai ◽  
...  
Keyword(s):  
Zinc Acetate ◽  
Dimethyl Carbonate ◽  
Reaction Pathway ◽  
Major Product ◽  
High Yield ◽  
Synthetic Route ◽  
Reaction Conditions ◽  
High Yields ◽  
By Products

The full N,N-methylation of 4,4′-methylenedianiline (MDA) with dimethyl carbonate (DMC) was investigated. The yield of the major product 4,4′-methylene bis(N,N-dimethylaniline) (MBDMA) reached as high as 97% over NaY catalyst at 190°C for 6 h. The catalyst could be used for two more times with acceptable MBDMA yields higher than 90%. The main by-products were identified as three N-methylated derivatives. Surprisingly, the formation of the N-methoxycarbonylation product was extremely restrained, which could be produced in high yields of 98% on zinc acetate catalyst. Furthermore, the reaction pathway to the major product MBDMA was proposed. Finally, a feasible synthetic route of 4,4′-methylene bis(N,N-dimethylaniline) (MBDMA) was established, featuring a high yield, mild reaction conditions, and simple operations.

scholarly journals Easy assembly of ligands for glycosidase affinity chromatography

1990 ◽  
Vol 270 (2) ◽  
pp. 539-540 ◽  
Author(s):  
R C Bernotas ◽  
B Ganem
Keyword(s):  
Amino Acids ◽  
Affinity Chromatography ◽  
Enzyme Purification ◽  
Reductive Amination ◽  
Water Soluble ◽  
High Yield ◽  
Glycosidase Inhibitors ◽  
Neutral Ph ◽  
Sepharose 4B ◽  
Derivatives Of

An improved, high-yield synthesis of the corresponding N-carboxypentyl derivatives of three iminoalditol glycosidase inhibitors has been developed for affinity chromatography enzyme purification. Reductive amination of 1-deoxynojirimycin (or its D-manno or D-galacto analogues) with methyl 5-formylvalerate and NaBH3CN at neutral pH afforted an aminoester which upon hydrolysis with aqueous 5% HCl gave the desired aminoacid in 97% overall yield. These amino acids could then be covalently attached using water-soluble carbodi-imide to 6-aminohexyl Sepharose 4B.

Energy-efficient synthesis of ferrite powders and films

2012 ◽  
Vol 1386 ◽  
Author(s):  
Ranajit Sai ◽  
Suresh D. Kulkarni ◽  
K. J. Vinoy ◽  
Navakanta Bhat ◽  
S. A. Shivashankar
Keyword(s):  
Energy Efficient ◽  
Water Soluble ◽  
Synthesis Methods ◽  
Efficient Synthesis ◽  
Microwave Assisted ◽  
Soft Chemical Synthesis ◽  
Reduce Energy Consumption ◽  
Post Synthesis ◽  
By Products ◽  
Significant Effort

ABSTRACTIn recent years, there has been significant effort in the synthesis of nanocrystalline spinel ferrites due to their unique properties. Among them, zinc ferrite has been widely investigated for countless applications. As traditional ferrite synthesis methods are energy- and time-intensive, there is need for a resource-effective process that can prepare ferrites quickly and efficiently without compromising material quality. We report on a novel microwave-assisted soft-chemical synthesis technique in the liquid medium for synthesis of ZnFe2O4 powder below 100 °C, within 5 min. The use of β-diketonate precursors, featuring direct metal-to-oxygen bonds in their molecular structure, not only reduces process temperature and duration sharply, but also leads to water-soluble and non-toxic by-products. As synthesized powder is annealed at 300 °C for 2 hrs in a conventional anneal (CA) schedule. An alternative procedure, a 2-min rapid anneal at 300 °C (RA) is shown to be sufficient to crystallize the ferrite particles, which show a saturation magnetization (MS) of 38 emu/g, compared with 39 emu/g for a 2-hr CA. This signifies that our process is efficient enough to reduce energy consumption by ∼85% just by altering the anneal scheme. Recognizing the criticality of anneal process to the energy budget, a more energy-efficient variation of the reaction process was developed, which obviates the need for post-synthesis annealing altogether. It is shown that the process also can be employed to deposit crystalline thin films of ferrites.

scholarly journals Analytical Characterization of Water-Soluble Constituents in Olive-Derived By-Products

Foods ◽  
2021 ◽  
Vol 10 (6) ◽  
pp. 1299
Author(s):  
Pablo Doménech ◽  
Aleta Duque ◽  
Isabel Higueras ◽  
José Luis Fernández ◽  
Paloma Manzanares
Keyword(s):  
Olive Tree ◽  
Mediterranean Area ◽  
Water Soluble ◽  
Olive Pomace ◽  
Olive Leaves ◽  
Olive Stone ◽  
Olive Trees ◽  
Tree Pruning ◽  
By Products

Olive trees constitute one of the largest agroindustries in the Mediterranean area, and their cultivation generates a diverse pool of biomass by-products such as olive tree pruning (OTP), olive leaves (OL), olive stone (OS), and extracted olive pomace (EOP). These lignocellulosic materials have varying compositions and potential utilization strategies within a biorefinery context. The aim of this work was to carry out an integral analysis of the aqueous extractives fraction of these biomasses. Several analytical methods were applied in order to fully characterize this fraction to varying extents: a mass closure of >80% was reached for EOP, >76% for OTP, >65% for OS, and >52% for OL. Among the compounds detected, xylooligosaccharides, mannitol, 3,4-dihydroxyphenylglycol, and hydroxytyrosol were noted as potential enhancers of the valorization of said by-products. The extraction of these compounds is expected to be more favorable for OTP, OL, and EOP, given their high extractives content, and is compatible with other utilization strategies such as the bioconversion of the lignocellulosic fraction into biofuels and bioproducts.

scholarly journals Multistep batch-flow hybrid synthesis of a terbinafine precursor

2021 ◽  
Author(s):  
Tamás Hergert ◽  
Béla Mátravölgyi ◽  
Róbert Örkényi ◽  
János Éles ◽  
Ferenc Faigl
Keyword(s):  
Methyl Ether ◽  
Lithium Salt ◽  
Scale Up ◽  
Hybrid Process ◽  
High Yield ◽  
Grignard Reaction ◽  
Efficient Synthesis ◽  
Synthetic Process ◽  
Synthesis Route ◽  
Selective Addition

AbstractA three-step batch-flow hybrid process has been developed for an expeditious synthesis of the enynol key intermediate of antifungal terbinafine. This procedure involves consecutive organometallic steps without the necessity of any in-line purification: after a metalation by n-butyllithium, a selective addition of the lithium salt was elaborated followed by a Grignard reaction resulting in a high yield of 6,6-dimethylhept-1-en-4-yn-3-ol. Moreover, as an alternative to tetrahydrofuran, cyclopentyl methyl ether was used as solvent implementing a safe, sustainable, yet selective synthetic process. Even on a laboratory-scale, the optimized batch-flow hybrid process had a theoretical throughput of 41 g/h. Furthermore, the newly developed process provides an efficient synthesis route to the key-intermediate, while making acrolein obsolete, minimizing side-products, and enabling safe and convenient scale-up.

Enantioselective synthesis of (R)-tolterodine using lithiation/borylation–protodeboronation methodology

2012 ◽  
Vol 90 (11) ◽  
pp. 965-974 ◽  
Author(s):  
Stefan Roesner ◽  
Varinder K. Aggarwal
Keyword(s):  
Enantioselective Synthesis ◽  
High Yield ◽  
Magnesium Bromide ◽  
Efficient Synthesis ◽  
Boronic Ester ◽  
Better Than

The synthesis of the pharmaceutical (R)-tolterodine is reported using lithiation/borylation–protodeboronation of a homoallyl carbamate as the key step. This step was tested with two permutations: an electron-neutral aryl Li-carbamate reacting with an electron-rich boronic ester and an electron-rich aryl Li-carbamate reacting with an electron-neutral boronic ester. It was found that the latter arrangement was considerably better than the former. Further improvements were achieved using magnesium bromide in methanol leading to a process that gave high yield and high enantioselectivity in the lithiation/borylation reaction. The key step was used in an efficient synthesis of (R)-tolterodine in a total of eight steps in a 30% overall yield and 90% ee.

scholarly journals Efficient Synthesis of Readily Water-Soluble Sulfonic Acid Carbamates

Molecules ◽  
2015 ◽  
Vol 20 (4) ◽  
pp. 6856-6865 ◽  
Author(s):  
Krzysztof Idzik ◽  
Karsten Nödler ◽  
Tobias Licha
Keyword(s):  
Sulfonic Acid ◽  
Water Soluble ◽  
Efficient Synthesis
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