反应详情

温度

20 °C

27 g of propyl chloroformate were slowly added to a mixture of 41.2 g of m-amino-3-methoxy-crotonanilide, 300 ml of tetrahydrofuran and 22.2 g of triethylamine and the mixture was stirred for 16 hours at 20° C. The mixture was filtered and the filtrate was evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with an 8- 2 methylene chloride-acetone mixture to obtain 40 g of m-(n-propyloxycarbonylamino)-3-methoxy-crotonanilide melting at 115° C. Crystallization from chloroform did not change the melting point.

1. filtrationThe mixture was filtered
2. customthe filtrate was evaporated to dryness under reduced pressure
3. customThe residue was chromatographed over silica gel
4. washwas eluted with an 8- 2 methylene chloride-acetone mixture