ABSTRACT
Mo(II) and W(II) compounds, Mo(η3-allyl)(CO)2(Tri-MEDA)Br (1), Mo(η3-allyl)(CO)2(TMEDA)Br (2), W(η3-allyl)(CO)2(Tri-MEDA)Br (3), and W(η3-allyl)(CO)2(TMEDA)Br (4) (Tri-MEDA = N,N,N'-trimethylethylenediamine), were synthesized and characterized. The molecular structures of 1 and 3 were nearly identical with a pseudo-octahedral geometry except for the different Mo and W metal centers. The thermogravimetric analysis of 1 and 3 showed approximately 53 and 64% residues at 550 °C, respectively, which were significantly higher than the values for the expected materials. However, 1 and 3 sublimed at 100 °C under 0.40 Torr and 120 °C under 0.50 Torr, respectively, confirming that they were volatile. For 1 and 3, the temperatures at a vapor pressure of 1 Torr and enthalpies of vaporization (ΔHvap) were 168.78 °C and 143.8 kJ mol-1, and 167.48 °C and 148.5 kJ mol-1, respectively. The tungsten compound (3) exhibited good durability for 5 weeks under a thermal stability test at a sublimation temperature of 120 °C.
ABSTRACT
Calpains are calcium-dependent proteases that cleave a variety of intracellular substrates. The overactivation of mu-calpain is associated with a wide range of disease conditions. To search for calpain inhibitors from natural products, the phytochemical constituents of the ethyl acetate fraction of the whole plant of Orostachys japonicus (Crassulaceae) were studied. The various chromatographic separation of this fraction led to the isolation of a new tannin, (-)-epicatechin 5-gallate (1) along with 9 known compounds. Their structures were elucidated by spectroscopic and chemical analyses. Among them, (-)-epicatechin 5-gallate (1) and kaempferol (9) exhibited moderate inhibitory activity against mu-calpain with IC(50) values of 18.0+/-2.9 and 15.4+/-2.0 microg/ml, respectively.