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Synthesis of Tin Steroids and the Relation between Structure and Anticancer Activity*
Published in Nate F. Cardarelli, Tin as a Vital Nutrient:, 2019
Triphenyltin hydroxide (3.67 g) and 4.265 g of cholic acid were dissolved in 100 mℓ of dry ethanol by heating the mixture in a beaker in a water bath or steam bath. The solution was transferred to a 125-mℓ round-bottomed flask fitted with a Soxhlet containing anhydrous calcium chloride. The Soxhlet was fitted with a reflux condenser through which ice-cold water was circulated. The mixture in the round-bottomed flask was heated until the solution boiled and the heater was adjusted to maintain a reflux cycle of about 20 min. The refluxing was continued for 6 hr. The mixture was then percolated through a 2-in. layer of a microsieve. It was then filtered and evaporated to one third of the volume. This concentrated solution was cooled in the refrigerator to obtain the crystals. These crystals were dissolved in hot, dry alcohol and further dried using magnesium perchlorate or calcium chloride, then recrystallized as before. The reaction is shown below:
Small Molecules: Process Intensification and Continuous Synthesis
Published in Anthony J. Hickey, Sandro R.P. da Rocha, Pharmaceutical Inhalation Aerosol Technology, 2019
Scale-up of batch reactions from the laboratory to the pilot plant and the manufacturing site has been the historical mode of operation for the pharmaceutical industry. Many of the operations conducted on pilot or manufacturing scales are performed on well-engineered equipment which has its basis of design in laboratory glassware such as a round-bottom flask, reflux condenser, and Buchner funnel. The reason for this is likely due to an attempt to replicate laboratory result and quickly scale chemistry from the laboratory into equipment of similar operation in order to produce API for use in clinical trials. The advantage of this for the industry has been clear in the past, namely, that this type of equipment is largely multifunctional, meaning that a variety of chemistry can be run in a typical pilot plant reactor train, and the equipment can be turned over between products relatively easily, albeit with occasional extended cleaning times.
Method of Extraction
Published in Ravindra Kumar Pandey, Shiv Shankar Shukla, Amber Vyas, Vishal Jain, Parag Jain, Shailendra Saraf, Fingerprinting Analysis and Quality Control Methods of Herbal Medicines, 2018
Ravindra Kumar Pandey, Shiv Shankar Shukla, Amber Vyas, Vishal Jain, Parag Jain, Shailendra Saraf
In this method, the material to be extracted is placed in a “thimble” made of cellulose or cloth in a central compartment with a siphoning device and side-arm, both of which are connected to a lower compartment. The solvent is placed in a lower compartment and a reflux condenser is attached above the central sample compartment. Note that each component of the set up (solvent container, sample compartment, and reflux condenser) is a separate item of glass ware which is assembled together with the appropriate contents to make the complete apparatus. The solvent in the lower container (usually a round-bottomed flask) is heated to boiling, and the vapor passes through the side-arm up into the reflux condenser. Here, the vapor liquefies and drips into the thimble containing the material to be extracted. The warm solvent percolates through the material and the wall of the thimble and the extract gradually collects in the central compartment. Once the height of the extract reaches the top of the siphon, the entire liquid in the central compartment flows through this and back into the lower solvent container (Figure 2.4). The process is then repeated (Subramanian et al., 2016).
Fabrication of a dual stimuli-responsive magnetic nanohydrogel for delivery of anticancer drugs
Published in Drug Development and Industrial Pharmacy, 2021
Bakhshali Massoumi, Rogayeh Mossavi, Sanaz Motamedi, Hossein Derakhshankhah, Somayeh Vandghanooni, Mehdi Jaymand
The DMAEMA and MA as vinyl monomers were grafted onto Fe3O4 NPs through a free radical ‘grafting from’ approach as follows. The MPS-Fe3O4 NPs (1.50 g) were dispersed in dried N,N-dimethylformamide (DMF, 50 ml) through sonication for 15 min followed by stirring for 1 h. Then, the DMAEMA (3 ml, 20 mmol) and MA (0.50 g, 5 mmol) monomers were added to the flask, and the flask was equipped with a reflux condenser. The reaction mixture was de-oxygenated by argon gas. At this time, the initiator (AIBN, 20 mg; 0.11 mmol) was added to the flask, and the reaction was proceeded at 80 °C for about 72 h under an inert atmosphere with continuous stirring. Afterward, the Fe3O4@P(DMAEMA-co-MA) core-shell NPs were collected by using a strong magnet bar, re-dispersed in DMF (50 ml), and isolated again to remove un-grafted polymeric chains or un-reacted monomers. Finally, the obtained NPs were dried under vacuum.
Green isolation and physical modification of pineapple stem waste starch as pharmaceutical excipient
Published in Drug Development and Industrial Pharmacy, 2019
Annisa Rahma, Melissa Adriani, Puji Rahayu, Raymond R. Tjandrawinata, Heni Rachmawati
The purity of the starch was evaluated by determining the total starch content according to ASEAN Manual of Food Analysis 2011 [17]. The sample was hydrolized with hydrochloric acid (3% v/v) using a reflux apparatus. The hydrolysate was cooled down, neutralized by sodium chloride, filtrated, and made up to 500 mL with deionized water. A 10 mL aliquot of the mixture was treated with Luff solution with the following condition: heating for 3 min using a heater, boiling for 10 min in a reflux condenser, and cooling on an ice bath. The solution was then mixed with sulfuric acid (25% w/v) and potassium iodide (20% w/v), followed by titration with thiosulfate as the titrant and copper blue as the indicator. The amount of sugars (glucose, fructose, and inverted sugar) was determined based on the volume of tiosulphate used in the titration. The total starch content was determined using Equation (1),