反应详情

温度

150 °C

A mixture of intermediate 19 (38.8 g), potassium acetae (20 g) and Pd/C (10%; 2 g) in CH3OH (500 ml) was stirred at 150° C. under 4.9×106 Pa (50 kg) pressure of CO, during 16 hours. The reaction mixture was cooled, filtered over dicalite, and the filtrate was evaporated. The residue was diluted with water, then extracted three times with DCM. The combined organic layers were dried, filtered and the solvent evaporated. The residue was dissolved in acetic acid (250 ml) and acetic anhydride (6 ml) was added dropwise. The mixture was stirred for 30 minutes at room temperature, then diluted with water (250 ml) and the resulting precipitate was filtered off, washed with water, then dried, yielding 19.4 g (64.7%) of methyl 7-(acetylamino)-1,3-benzodioxole-4-carboxylate (intermediate 20).

1. temperatureThe reaction mixture was cooled
2. filtrationfiltered over dicalite
3. customthe filtrate was evaporated
4. additionThe residue was diluted with water
5. extractionextracted three times with DCM
6. customThe combined organic layers were dried
7. filtrationfiltered
8. customthe solvent evaporated
9. dissolutionThe residue was dissolved in acetic acid (250 ml)
10. additionacetic anhydride (6 ml) was added dropwise
11. stirringThe mixture was stirred for 30 minutes at room temperature
12. additiondiluted with water (250 ml)
13. filtrationthe resulting precipitate was filtered off
14. washwashed with water
15. customdried