Synthesis of Thieno23-d-13-dithiol-2-thiones from Thieno23-d-123-thiadiazoles: Matryoshka-type autoclave for high-temperature high-pressure thermolysis microscale reactions

摘要

Thieno[2,3-d]-1,2,3-thiadiazoles (>1) react with carbon disulfide in a "Matryoshka-type" double compartment autoclave [] to yield thieno[2,3-d]-1,3-dithiol-2-thiones (>2). With BH3/Me2S the cyclic trithiocarbonate (>2d) is cleaved and the product characterized after methylation as >4b. Compounds >7a and >7b are prepared via the thieno[2,3-d]-1,3-dithiolium salts (>6) followed by NaBH4-reduction.