Analytical approach for lubricant characterization of excipients using the surface replication method.

Lubricants are indispensable pharmaceutical ingredients for preventing tableting failure due to powder adhesion to the die wall. The impact of lubricants was evaluated with use of the Binding Identification for Net Detriment (BIND) surface replication method. Raloxifene hydrochloride (RH) was selected as a model chemical with high adhesion, and four commercially available tablet lubricants - stearic acid, sodium stearyl fumarate, calcium stearate, and magnesium stearate - were used for RH formulation.

BIND, a novel analytical approach for monitoring powder adhesion at the die wall with use of the surface replication method.

Tableting failure due to binding is often caused by powder adhesion to the die wall. The present study was undertaken to develop a novel approach for analyzing the binding characteristics of various formulations and manufacturing methods, named "Binding Identification for Net Detriment" (BIND). Binding characteristics with raloxifene hydrochloride as a model preparation were evaluated by visual observation, ejection force and BIND.

Formulation design of granules prepared by wet granulation method using a multi-functional single-punch tablet press to avoid tableting failures.

We previously determined "Tableting properties" by using a multi-functional single-punch tablet press (GTP-1). We plotted "Compactability" on the x-axis against "Manufacturability" on the y-axis to allow visual evaluation of "Tableting properties". Here, we examined whether this evaluation method can be used in the formulation design of tablets prepared by wet granulation.

Prediction of effects of punch shapes on tableting failure by using a multi-functional single-punch tablet press.

We previously determined "Tableting properties" by using a multi-functional single-punch tablet press (GTP-1). We proposed plotting "Compactability" on the x-axis against "Manufacturability" on the y-axis to allow visual evaluation of "Tableting properties". Various types of tableting failure occur in commercial drug production and are influenced by the amount of lubricant used and the shape of the punch.

Characterization of tableting properties measured with a multi-functional compaction instrument for several pharmaceutical excipients and actual tablet formulations.

Before designing tablet formulations, it is important to understand the "Tableting Properties" of excipients and API (active pharmaceutical ingredient) powders. Those properties refer to "Compressibility", "Compactability" and "Manufacturability", which are difficult to evaluate quantitatively. In this study, we aimed to evaluate the "Tableting Properties" by using a benchtop single-punch tablet press, developed recently to measure these parameters using a single device.

Asymmetric tandem Michael-aldol reactions between 3-cinnamoyloxazolidine-2-thiones and aldehydes.

Reactions between chiral 3-cinnamoyl-4-methyl-5-phenyl-1,3-oxazolidine-2-thiones and aromatic aldehydes in the presence of BF3Et2O diastereoselectively produced tricyclic compounds incorporating a bridgehead carbon bound to four heteroatoms in high yields. Four stereocenters were induced during the reaction. The tricyclic products were transformed into propane-1,3-diols bearing three consecutive stereocenters by acid hydrolysis, S-methylation, and reductive removal of the chiral auxiliary.

Chalcogeno-Morita-Baylis-Hillman reaction of enones with acetals: simple alpha-alkoxyalkylation of enones.

1-[2-(Methylsulfanyl)phenyl]prop-2-en-1-one (1) and the seleno congener (2) reacted with acetals 3 and 21 in the presence of BF(3).Et(2)O to give alpha-alkoxyalkyl enones 4, 5 and 22, 23 in good yields. When the reaction mixtures were worked up with a saturated NaHCO(3) solution instead of Et(3)N, onium salts 6 and 7 were obtained together with 4 and 5.