Natural Product Chemistry, ‡Centre for Nuclear Magnetic Resonance, §Laboratory of X-ray Crystallography, Indian Institute of Chemical Technology , Hyderabad 500 007, India.
J Org Chem. 2013 Jun 21;78(12):6303-8. doi: 10.1021/jo400680w. Epub 2013 May 28.
A novel thia-Prins bicyclization approach has been developed for the first time for the synthesis of hexahydro-2H-thieno[3,2-c]thiopyran derivatives from the coupling of homoallylic mercaptans such as hex-3-ene-1,6-dithiol with various aldehydes using 10 mol % InBr3 in dichloromethane with high selectivity. In addition, the coupling of (E)-N-(6-mercaptohex-3-enyl)-4-methylbenzenesulfonamide with aldedydes affords the corresponding N-tosyloctahydrothiopyrano[4,3-b]pyrrole derivatives in good yields. This reaction is a stereoselective affording trans-fused product from E-homoallyllic mercaptan and cis-fused product from Z-homoallyllic mercaptan.
首次开发了一种新型的噻-Prins 双环化方法,用于从偕丙基硫醇(如己-3-烯-1,6-二硫醇)与各种醛的偶联,以高选择性合成六氢-2H-噻吩并[3,2-c]噻喃衍生物,使用 10 mol % InBr3 在二氯甲烷中。此外,(E)-N-(6-巯基己-3-烯基)-4-甲基苯磺酰胺与醛的偶联以良好的收率得到相应的 N-对甲苯磺酰基八氢噻吩并[4,3-b]吡咯衍生物。该反应是立体选择性的,从 E-偕丙基硫醇得到反式稠合产物,从 Z-偕丙基硫醇得到顺式稠合产物。