反应详情

温度

60 °C

A reactor was charged with 1c (16.0 g), Pd/C (2.08 g), anhydrous Na2CO3 (2.56 g) and ethyl acetate (120 mL). The flask was vacuum-purged with nitrogen (3×) and vacuum-purged with hydrogen (3×). The flask was then pressurized with hydrogen and stirred at about 60° C. until completion of reaction. The flask was cooled to 20-25° C., the pressure released to ambient, the head space purged with nitrogen three times and mixture was filtered. The filtrate was concentrated. Methanol was added. The mixture was stirred and then cooled. Product precipitated and was filtered and dried in an oven (Yield: 90%, HPLC: 99.7%).

1. customThe flask was vacuum-purged with nitrogen (3×)
2. customvacuum-purged with hydrogen (3×)
3. temperatureThe flask was cooled to 20-25° C.
4. customthe head space purged with nitrogen three times and mixture
5. filtrationwas filtered
6. concentrationThe filtrate was concentrated
7. additionMethanol was added
8. stirringThe mixture was stirred
9. temperaturecooled
10. customProduct precipitated
11. filtrationwas filtered
12. customdried in an oven (Yield: 90%, HPLC: 99.7%)