反应详情

25 g (81.6 mmol) of dithiodibenzoic acid is refluxed in 60 ml of SOCl2 and 1.5 ml of dimethylformamide (DMF) for 3 hrs. Then the excess of SOCl2 is distilled off, and the residue is dissolved in CHCl3 and added dropwise to a solution of methanol (50 ml) and triethylamine (0.204 mol) in CHCl3 (300 l). After standing over night the reaction mixture is shaked with water and saturated K2CO3 solution. After drying the organic layer the solvent is evaporated and methanol is added to the residue (oil). 13.6 g (50%) of solid product is obtained.

1. distillationThen the excess of SOCl2 is distilled off
2. dissolutionthe residue is dissolved in CHCl3
3. waitAfter standing over night
4. customAfter drying the organic layer the solvent
5. customis evaporated
6. additionmethanol is added to the residue (oil)