(+/-)-2-Thienylcarbinols and their O-acetyl derivatives were resolved in re
verse separation by CCL and PLE catalysed hydrolysis to afford optically ac
tive 2-thienylcarbinols in 35%-99% e.e. that are valuable chiral building b
locks, in particular in the synthesis of pheromones and some alkoloid type
natural products. Absolute configurations were determined by the correlatio
n of specific rotation values with the literature and by transforming into
the corresponding secondary alcohols via reductive desulfurization by Ra-Ni
.