反应详情

温度

27.5 °C

To 1.98 g (+)-Methyl (2-chlorophenyl)-(6,7-dihydro-4H-thieno[3,2-c]pyrid-5-yl)acetate was added 5 mL of acetone and stirred at 25-30° C. The temperature of the reaction mixture was raised from 25 to 50-52° C. and within one lot 0.7 g of concentrated H2SO4 (95%) was added with constant stirring and the reaction mixture was suddenly cooled to 0° C. to −5° C. for 10 min. Later the reaction mixture was stirred at 25-30° C. for 12 hrs, the thick precipitate obtained was filtered, washed with 5 mL of acetone and the residue (1.6 g, 62%) was dried in a vacuum oven.

1. additionwas added
2. stirringwith constant stirring
3. temperaturethe reaction mixture was suddenly cooled to 0° C. to −5° C. for 10 min
4. stirringLater the reaction mixture was stirred at 25-30° C. for 12 hrs
5. customthe thick precipitate obtained
6. filtrationwas filtered
7. washwashed with 5 mL of acetone
8. dry with materialthe residue (1.6 g, 62%) was dried in a vacuum oven