The utilisation of the 2-cyanoethyl group as a versatile protecting group for 2-thioxo-1, 3- dithiole-4, 5-dithiolates and tetrathiafulvalene-thiolates is reported. Mono deprotection of bis- protected 2-thi-oxo-1, 3-dithiole-4, 5-dithiolate and of bis-protected tetrathiafulva-lene-2, 3- dithiolates [obtained by cross coupling of 4, 5-bis (2-cyano-ethylthio)-1, 3-dithio-2-one 5 and the 1, 3-dithiole-2-thiones 2b—h and 2 j in triethyl phosphite] was achieved in very high ...