反应详情

0.38 moles of sulfuryl chloride in an equal volume of carbon tetrachloride was added dropwise to 21.6 gm (0.11 moles) of 2-(3-methylphenyl)-1,3-dithiolane dissolved in 22 mls of carbon tetrachloride while refluxing and stirring. After the addition, the reaction mixture was stirred for 1 hour at reflux and allowed to cool to room temperature. The solvent was evacuated and the residue Kugelrohr distilled at 65°-70° C. (0.43 mm/Hg) to give 18.32 gm (89.9% yield) of product. NMR and Gas Chromatograph/Mass Spectrometry (GC/MS) Analysis: 1H--NMR (CCl4) δ2.27 (S, CH3), 6.9 to 7.2 and 7.5 to 7.65 (m+ 4H, aryl protons); GCMS (70 ev), M/e (% rel. int.) 212 (M +4, 4), 210 (M+ +2, 12), 208 (M+, 13), 177 (13), 175 (79), 173 (100), 138 (15), 103 (26), 102 (25), 101 (19), 87 (20), 86 (16), 77 (23), 75 (19), 69 (22), 68 (24), 51 (64).

1. temperaturewhile refluxing
2. additionAfter the addition
3. stirringthe reaction mixture was stirred for 1 hour
4. temperatureat reflux
5. customThe solvent was evacuated
6. distillationthe residue Kugelrohr distilled at 65°-70° C. (0.43 mm/Hg)