scholarly journals A Novel Telescoped Kilogram-Scale Process for Preparation of Obeticholic Acid

2021 ◽  
Vol 03 (02) ◽  
pp. e56-e64
Author(s):  
Cheng-Wei Li ◽  
Cai Wang ◽  
Chao Guo ◽  
Bin-Hua Lv ◽  
You-Fu Luo
Keyword(s):  
Environmentally Friendly ◽  
Scale Production ◽  
Obeticholic Acid ◽  
One Pot ◽  
Ketone Reduction ◽  
Step Process ◽  
Amide Hydrolysis ◽  
Work Up ◽  
Final Purification

A novel scalable four-step process has been developed to improve the synthesis of obeticholic acid (OCA). The key step of this process was the isolation of the amide intermediate, which underwent hydrogenation, basic epimerization, ketone reduction, and amide hydrolysis in a one-pot procedure. The use of efficient single recrystallization for the final purification in this process made the corresponding work-up procedure more concise and environmentally friendly. A kilogram-scale production of OCA following this process could achieve over 70% yield with all impurities controlled below 0.10%.

Synthesis of Eco-Friendly High PL Lifespan Manganese-Doped CuInZnS/ZnS QDs for White LED Applications

2020 ◽  
Vol 20 (10) ◽  
pp. 6286-6294
Author(s):  
Mukerem Helil Abib ◽  
Taotao Chen ◽  
Enze Xu ◽  
Man Wang ◽  
Yang Jiang
Keyword(s):  
White Light ◽  
Surface Passivation ◽  
Environmentally Friendly ◽  
White Led ◽  
One Pot ◽  
Step Process ◽  
The One ◽  
Mn Doped

Environmentally friendly and long PL lifespan Mn-doped CuInZnS (Mn:CIZS) and CuInZnS/ZnS (Mn:CIZS/ZnS) QDs, with respective red and yellow emissions, were synthesized using nontoxic precursors via a facile dual-step process based on the one-pot method. The resulting Mn:CIZS and Mn:CIZS/ZnS QDs exhibited confirmed strong red and yellow photoluminescence emissions at approximately 654 nm and 580 nm, respectively. The measured PL decay lifespan for the Mn: CIZS QDs is 2.52 μs due to well-organized surface passivation through the ZnS shell; the average PL lifespan for the Mn:CIZS/ZnS QDs is extended to 6.28 μs. Moreover, the WLEDs were composed of the Mn:CIZS/ZnS QDs. The resulting WLEDs offered admirable optical attributes, such as an excellent Ra of 89, a low Tc of 5075 K and radiant white light emanation at 60 mA functional current. Therefore, the outputs highlight the Mn:CIZS/ZnS QDs as hopeful cadmium-free resources for the interest of optoelectronics exploration.

A Clean One-pot Synthesis of 7-Amino-5-Aryl-6-Cyano-1,5-Dihydro-2H-Pyrano[2,3-d] Pyrimidine-2,4(3H)-Diones in Aqueous Media under Ultrasonic Irradiation

2005 ◽  
Vol 2005 (3) ◽  
pp. 162-163 ◽  
Author(s):  
Tong-Shou Jin ◽  
Li-Bin Liu ◽  
Ying Zhao ◽  
Tong-Shuang Li
Keyword(s):  
Ultrasonic Irradiation ◽  
Aqueous Media ◽  
Environmentally Friendly ◽  
Green Solvent ◽  
One Pot ◽  
One Pot Synthesis ◽  
Novel Approach ◽  
Work Up

A novel approach to the synthesis of 7-amino-5-aryl-6-cyano-1,5-dihydro-2H-pyrano[2,3-d]pyrimidine-2,4(3H)-diones in aqueous media under ultrasonic irradiation without catalyst is described. This method provides several advantages such as being environmentally friendly, simple work-up procedure and milder condition. In addition, water was chosen as a green solvent.

scholarly journals Toward a Practical, Two-Step Process for Molnupiravir from Cytidine

2021 ◽  
Author(s):  
Dinesh J. Paymode ◽  
Natarajan Vasudevan ◽  
Saeed Ahmad ◽  
Appasaheb L. Kadam ◽  
Flavio S. P. Cardoso ◽  
...  
Keyword(s):  
Total Concentration ◽  
Primary Alcohol ◽  
Environmentally Friendly ◽  
Active Pharmaceutical Ingredient ◽  
Crystalline Hydrate ◽  
Step Process ◽  
Work Up

<p>A two-step synthesis of molnupiravir (<b>1</b>) is presented. This work focuses on the development of practical reaction and purification conditions toward a manufacturing route. The sequence commences from highly available cytidine (<b>2</b>), and molnupiravir is formed through direct hydroxamination of the cytosine ring and esterification of the sugar’s primary alcohol without use of protecting or activating groups. A highly crystalline hydrate of <i>N</i>-hydroxycytidine (<b>3</b>) resulted in an easily purified intermediate, and a practical, off-the-shelf enzyme was selected for the acylation. The yield was increased through a chemically-promoted, selective ester cleavage which converted a by-product, molnupiravir isobutyryl oxime ester (<b>4</b>), into the final API. Both reactions proceed in >90% assay yield and crystallization procedures are used to afford intermediate and active pharmaceutical ingredient in purities above 99% with an overall yield of 60%. Excellent throughput and sustainability is achieved by limiting the total concentration to 7 volumes of solvent in the course of the two reactions with an overall PMI of 41 including work-up and isolation. Environmentally friendly solvents, water and 2-methyl tetrahydrofuran, enhance sustainability of the operation. </p>

scholarly journals Toward a Practical, Two-Step Process for Molnupiravir from Cytidine

2021 ◽  
Author(s):  
Dinesh J. Paymode ◽  
Natarajan Vasudevan ◽  
Saeed Ahmad ◽  
Appasaheb L. Kadam ◽  
Flavio S. P. Cardoso ◽  
...  
Keyword(s):  
Total Concentration ◽  
Primary Alcohol ◽  
Environmentally Friendly ◽  
Active Pharmaceutical Ingredient ◽  
Crystalline Hydrate ◽  
Step Process ◽  
Work Up

<p>A two-step synthesis of molnupiravir (<b>1</b>) is presented. This work focuses on the development of practical reaction and purification conditions toward a manufacturing route. The sequence commences from highly available cytidine (<b>2</b>), and molnupiravir is formed through direct hydroxamination of the cytosine ring and esterification of the sugar’s primary alcohol without use of protecting or activating groups. A highly crystalline hydrate of <i>N</i>-hydroxycytidine (<b>3</b>) resulted in an easily purified intermediate, and a practical, off-the-shelf enzyme was selected for the acylation. The yield was increased through a chemically-promoted, selective ester cleavage which converted a by-product, molnupiravir isobutyryl oxime ester (<b>4</b>), into the final API. Both reactions proceed in >90% assay yield and crystallization procedures are used to afford intermediate and active pharmaceutical ingredient in purities above 99% with an overall yield of 60%. Excellent throughput and sustainability is achieved by limiting the total concentration to 7 volumes of solvent in the course of the two reactions with an overall PMI of 41 including work-up and isolation. Environmentally friendly solvents, water and 2-methyl tetrahydrofuran, enhance sustainability of the operation. </p>

An Efficient and Improved Process for the Synthesis of Itopride Hydrochloride and Trimethobenzamide Hydrochloride

2018 ◽  
Vol 15 (4) ◽  
pp. 572-575 ◽  
Author(s):  
Ponnusamy Kannan ◽  
Samuel I.D. Presley ◽  
Pallikondaperumal Shanmugasundaram ◽  
Nagapillai Prakash ◽  
Deivanayagam Easwaramoorthy
Keyword(s):  
Large Scale ◽  
Hydroxylamine Hydrochloride ◽  
Scale Production ◽  
One Pot ◽  
Hydrochloride Salt ◽  
Environmental Friendly ◽  
Large Scale Production ◽  
Non Ulcer Dyspepsia ◽  
Itopride Hydrochloride ◽  
Yield And Purity

Aim and Objective: Itopride is a prokinetic agent used for treating conditions like non-ulcer dyspepsia. Itopride is administered as its hydrochloride salt. Trimethobenzamide is used for treating nausea and vomiting and administered as its hydrochloride salt. The aim is to develop a novel and environmental friendly method for large-scale production of itopride and trimethobenzamide. Materials and Methods: Itopride and trimethobenzamide can be prepared from a common intermediate 4- (dimethylaminoethoxy) benzyl amine. The intermediate is prepared from one pot synthesis using Phyrdroxybenzaldehye and zinc dust and further reaction of the intermediate with substituted methoxy benzoic acid along with boric acid and PEG gives itopride and trimethobenzamide. Results: The intermediate 4-(dimethylaminoethoxy) benzylamine is prepared by treating p-hydroxybenzaldehyde and 2-dimethylaminoethyl chloride. The aldehyde formed is treated with hydroxylamine hydrochloride. The intermediate is confirmed by NMR and the purity is analysed by HPLC. Conclusion: Both itopride and trimethobenzamide were successfully synthesized by this method. The developed method is environmental friendly, economical for large-scale production with good yield and purity.

scholarly journals Aqueous one-pot synthesis of well-defined zwitterionic diblock copolymers by RAFT polymerization: an efficient and environmentally-friendly route to a useful dispersant for aqueous pigments

2021 ◽  
Vol 23 (3) ◽  
pp. 1248-1258
Author(s):  
Shannon M. North ◽  
Steven P. Armes
Keyword(s):  
Iron Oxide ◽  
Diblock Copolymers ◽  
Raft Polymerization ◽  
Environmentally Friendly ◽  
Iron Oxide Particles ◽  
One Pot ◽  
One Pot Synthesis ◽  
Highly Effective ◽  
Oxide Particles

An atom-efficient, wholly aqueous one-pot synthesis of zwitterionic diblock copolymers has been devised. Such copolymers can serve as highly effective aqueous dispersants for nano-sized transparent yellow iron oxide particles.

Vegetable oil as a highly effective 100% bio-based alternative solvent for the one-pot multicomponent Biginelli reaction

2021 ◽  
Author(s):  
Pakin Noppawan ◽  
Suwiwat Sangon ◽  
Nontipa Supanchaiyamat ◽  
Andrew J. Hunt
Keyword(s):  
Vegetable Oil ◽  
Palm Oil ◽  
Biginelli Reaction ◽  
Environmentally Friendly ◽  
One Pot ◽  
Highly Effective ◽  
The One ◽  
Biginelli Reactions

Multicomponent one-pot Biginelli reactions have been successfully performed using vegetable oil as bio-based, non-toxic, and environmentally friendly solvents. Palm oil was demonstrated to be a highly effective greener solvent as...

scholarly journals One-Pot Synthesis of 7, 7-Dimethyl-4-Phenyl-2-Thioxo-2,3,4,6,7, 8-Hexahydro-1H-Quinazoline-5-OnesUsing Zinc Ferrite Nanocatalyst and Its Bio Evaluation

Catalysts ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 431
Author(s):  
Tentu Nageswara Rao ◽  
Nalla Krishnarao ◽  
Faheem Ahmed ◽  
Suliman Yousef Alomar ◽  
Fadwa Albalawi ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Zinc Ferrite ◽  
Large Scale ◽  
Cyano Group ◽  
Proton Nuclear Magnetic Resonance ◽  
Scale Production ◽  
One Pot ◽  
Antibacterial And Antifungal ◽  
Nuclear Magnetic

A simple and highly efficient protocol for the synthesis of derivatives 7, 7-dimethyl-4-phenyl-2-thioxo-2, 3, 4, 6, 7, 8-hexahydro-1H-quinazoline-5-one from 5, 5-dimethyl cyclohexane-1, 3-dione (4a–4h) (dimedone) has been described. The aryl aldehydes were substituted with thiourea in the presence of synthesized zinc ferrite nanocatalyst, which increased the yield under reflux through condensation, followed by cyclization to give desired products. The other advantages are that it is eco-friendly and economically affordable for large-scale production. Structural validation and characterization of all the newly synthesized compounds were evaluated by spectral analysis (mass spectrometry, proton nuclear magnetic resonance (1HNMR), and Carbon-13 nuclear magnetic resonance(13CNMR)spectroscopies. The structure of antibacterial and antifungal assays was performed with the newly synthesized compounds. The antimicrobial activity of title compounds possessing electron-withdrawing groups such as (4e–4h) (Cl, Br, and cyano group) exhibited more active potential than the electron-donating groups, C6H5,4-C6H4, 3-OC2H5-4OH-C6H3, etc., (4a–4d) containing moiety.

Rapid and Green One-Pot Synthesis of Novel 2-(4-Hydroxy-2-oxo-2H-chromen-3-yl)-2-(arylamino)-1H-indene-1,3(2H)-diones

2021 ◽  
Vol 18 ◽  
Author(s):  
Abolfazl Olyaei ◽  
Zahra Ghahremany ◽  
Madieh Sadeghpour
Keyword(s):  
Aromatic Amines ◽  
Low Cost ◽  
Guanidine Hydrochloride ◽  
Reaction Times ◽  
Solvent Free ◽  
One Pot ◽  
Solvent Free Conditions ◽  
The One ◽  
High Yields ◽  
Work Up

: A green and efficient protocol was developed for the one-pot three-component synthesis of novel 2-(4-hydroxy-2-oxo-2H-chromen-3-yl)-2-(arylamino)-1H-indene-1,3(2H)-dione derivatives by the reaction of 4-hydroxycoumarin, ninhydrin and aromatic amines in the presence of guanidine hydrochloride as an organocatalyst under solvent-free conditions. The present approach offers several advantages such as low cost, simple work-up, short reaction times, chromatography-free purification, high yields and greener conditions.

One-pot synthesis of gold nanoparticles embedded in polysaccharide-based hydrogel: Physical-chemical characterization and feasibility for large-scale production

2019 ◽  
Vol 124 ◽  
pp. 838-845 ◽  
Author(s):  
Morgana Souza Marques ◽  
Κarine Modolon Zepon ◽  
Julia Maia Heckler ◽  
Fernando Dal Pont Morisso ◽  
Marcos Marques da Silva Paula ◽  
...  
Keyword(s):  
Gold Nanoparticles ◽  
Large Scale ◽  
Chemical Characterization ◽  
Scale Production ◽  
One Pot ◽  
One Pot Synthesis ◽  
Physical Chemical ◽  
Large Scale Production
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