反应详情

To an ice-cooled mixture of the Compound 3a (5.00 g, 25.6 mmol) and propane-1,3-dithiol (2.92 g, 27 mmol) in chloroform (75 mL) was added boron trifluoride etherate (2 mL). The mixture was stirred and allowed to warm to room temperature. After stirring for 3 hours, most of the solid had dissolved. Magnesium sulfate was added to dry the solution, and stirring was continued overnight. Filtration and evaporation of the solvent afforded a light yellow solid. This material was triturated with butyl chloride to give the Compound 3b; m.p. 192°-194° C.; 1H NMR (CDCl3 +MeSO-d6 +D2O) δ1.8-2.3 (m, 2H, CH2CH2CH2), 2.9-3.2 (m, 4H, --CH2CH2CH2 --), 6.56 (s, 1H, --SCHS--), 7.6-8.8 (m, 3H, ArH).

1. stirringAfter stirring for 3 hours, most of the solid
2. dissolutionhad dissolved
3. customto dry the solution
4. stirringstirring
5. filtrationFiltration and evaporation of the solvent
6. customafforded a light yellow solid
7. customThis material was triturated with butyl chloride