反应详情

0.35 mol (32 mL) of POCl3 was added at 0° C. to a 1.0 mol (77 mL) of DMF (excess of DMF used as solvent). At the end of the addition, the mixture was allowed to warm to room temperature and stirred for 1 h. Then it was cooled again to 0° C. and treated with 3-methyl-2-phenylthiophene (60 g, 0.35 mol). The resulting reaction mixture was allowed to reach room temperature and after 12 h stirring at the same temperature was heated at 80° C. for 2 days. Then it was poured into a mixture of ice and water, added of sodium acetate and extracted with CHCl3 (3×150 mL). The organic phase was separated, washed with water until neutral pH, dried over MgSO4 and evaporated off to dryness. The residue was crystallized. Yield 60.2 g (85%).

1. additionAt the end of the addition
2. temperatureThen it was cooled again to 0° C.
3. customThe resulting reaction mixture
4. waitto reach room temperature and after 12 h
5. stirringstirring at the same temperature
6. temperaturewas heated at 80° C. for 2 days
7. extractionextracted with CHCl3 (3×150 mL)
8. customThe organic phase was separated
9. washwashed with water until neutral pH
10. dry with materialdried over MgSO4
11. customevaporated off to dryness
12. customThe residue was crystallized