Computational Approach to Solvent-Free Synthesis of Ethyl Oleate UsingCandidarugosaandCandidaantarctica BLipases. I. Interfacial Activation and Substrate (Ethanol, Oleic Acid) Adsorption

2004 ◽  
Vol 5 (6) ◽  
pp. 2366-2375 ◽  
Author(s):  
M. Laura Foresti ◽  
M. Luján Ferreira
Keyword(s):  
Oleic Acid ◽  
Ethyl Oleate ◽  
Computational Approach ◽  
Solvent Free ◽  
Interfacial Activation ◽  
Solvent Free Synthesis

Room Temperature Solvent-Free Synthesis of Monodisperse Magnetite Nanocrystals

2006 ◽  
Vol 6 (3) ◽  
pp. 852-856 ◽  
Author(s):  
X. R. Ye ◽  
C. Daraio ◽  
C. Wang ◽  
J. B. Talbot ◽  
S. Jin
Keyword(s):  
Oleic Acid ◽  
Solid State ◽  
Large Scale ◽  
Room Temperature ◽  
Solvent Free ◽  
Two Dimensional ◽  
New Process ◽  
High Boiling Point ◽  
Magnetite Nanocrystals ◽  
Solvent Free Synthesis

We have successfully demonstrated a facile, solvent-free synthesis of highly crystalline and monodisperse Fe3O4 nanocrystallites at ambient temperature avoiding any heating. Solid state reaction of inorganic Fe(II) and Fe(III) salts with NaOH was found to produce highly crystalline Fe3O4 nanoparticles. The reaction, if carried out in the presence of surfactant such as oleic acid–oleylamine adduct, generated monodisperse Fe3O4 nanocrystals extractable directly from the reaction mixture. The extracted nanoparticles were capable of forming self-assembled, two-dimensional and uniform periodic array. The new process utilizes inexpensive and nontoxic starting materials, and does not require a use of high boiling point and toxic solvents, thus is amenable to an environmentally desirable, large-scale synthesis of nanocrystals.

Temperature Dependent Green Synthesis of 3-Carboxycoumarins and 3,4-unsubstituted Coumarins

2019 ◽  
Vol 16 (1) ◽  
pp. 130-135 ◽  
Author(s):  
Jack van Schijndel ◽  
Dennis Molendijk ◽  
Luiz Alberto Canalle ◽  
Erik Theodorus Rump ◽  
Jan Meuldijk
Keyword(s):  
Knoevenagel Condensation ◽  
Ammonium Bicarbonate ◽  
Solvent Free ◽  
Temperature Dependent ◽  
Step Procedure ◽  
Synthetic Routes ◽  
High Yields ◽  
Temperature Optima ◽  
Solvent Free Synthesis ◽  
Full Conversion

Aim and Objective: Because of the low abundance of 3,4-unsubstituted coumarins in plants combined with the complex purification process required, synthetic routes towards 3,4-unsubstituted coumarins are especially valuable. In the present work, we explore the possibilities of a solvent-free Green Knoevenagel condensation on various 2-hydroxybenzaldehyde derivatives and malonic acid without the use of toxic organocatalysts like pyridine and piperidine but only use ammonium bicarbonate as the catalyst. Materials and Methods: To investigate the scope of the Green Knoevenagel condensation for the synthesis of 3,4-unsubstituted coumarins, various 2-hydroxybenzaldehyde derivatives were screened as starting material in the optimized two-step procedure developed for 2-hydroxybenzaldehyde. </P><P> Results: This study shows that the intramolecular esterification and the decarboxylation are in competition, but show different temperature optima. In order to suppress premature decarboxylation and maximize the yield of coumarin, a two-step procedure was adopted. The reaction mixture containing ammonium bicarbonate is initially kept at 90ºC for 1 hour. After completion of the cyclization, the temperature of the reaction mixture is increased to 140ºC for 2 hours. Following this protocol, coumarin could be isolated with a yield of 95%. Conclusion: A two-step procedure for the solvent-free synthesis of several 3,4-unsubstituted coumarins was developed using ammonium bicarbonate, resulting in high yields of the desired products. Moreover, this procedure has a low E-factor and is, therefore an environmental friendly reaction in line with the principles of Green Chemistry. It was shown that by initially capping the temperature at 90ºC, premature decarboxylation can be suppressed. After full conversion to the intermediate 3-carboxycoumarin, the temperature can be increased to 140ºC finalizing the reaction. Ammonium bicarbonate was shown to catalyze both the Green Knoevenagel condensation and the decarboxylation step.

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