An improved method is described for preparation of thiolcrotonates by reaction of crotonyl chloride with thiols. General convenient and high-yield methods of making the new dl-3- chlorothiolbutyrates and the new dl-3-alkyl (aryl) thiothiolbutyrates involve addition of hydrogen chloride and of thiols, respectively, to thiolcrotonates. General procedures for making thiolesters by esterification of thiols with anhydride8 involve use of 1 mole of ...