反应详情

温度

35 °C

(±)-2-(2-Chlorophenyl)-(6,7-dihydro-4H-thieno[3,2-c]pyrid-5-yl)acetonitrile (713 g; 2.46 mol) was added to methanol (3.505 l) at 23-28° C. with stirring. To this slurry, potassium carbonate (170 g; 1.23 mol) was added followed by dimethyl sulfoxide (263 ml; 3.7 mol). The contents were heated between 30-40° C. and 30.0% aqueous hydrogen peroxide solution (382 ml; 3.70 mol) was added between 40-50° C. slowly over a period of 3 hours. After the addition was over, the reaction mixture was maintained at this temperature for a further 2 hours, after which the reaction was brought to 20-30° C. 35% Hydrochloric acid (213.0 ml) in water (10.7 l) was added slowly to the reaction mixture over a period of 1 hour 15 minutes. After stirring for 1 hour, the solid formed was filtered and washed with a 1:1 methanol: water mixture (3.565 l). The isolated solid was dried in a vacuum oven at 75-80° C. for a period of 12 hours. Yield: 716 g (94.72%). mp: 124-126° C. The product was identified by IR spectrum, 1H and 13C NMR investigation.

1. additionAfter the addition
2. temperaturewas maintained at this temperature for a further 2 hours
3. customwas brought to 20-30° C
4. stirringAfter stirring for 1 hour
5. customthe solid formed
6. filtrationwas filtered
7. washwashed with a 1:1 methanol
8. customThe isolated solid was dried in a vacuum oven at 75-80° C. for a period of 12 hours