反应详情

A stirred solution of the product from example 85 (11.01 g, 21.03 mmol) in 180 mL ethyl acetate (180 mL) was treated with a 1N HCl/ethyl acetate (21 mL) solution at ambient temperature. The resulting slurry was stirred for approximately 1 hour at room temperature. The slurry was pressure filtered under nitrogen through a stainless steel filter. The filter cake was washed three times with ethyl acetate (30 mL) and dried under a nitrogen purge for 2 hours. The filter cake was then dried in a vacuum oven at 60° C. overnight. This afforded 10.46 g (88.8%) of product as a white solid. EA: Calculate for C32H34ClN3O4: C 68.63, H 6.12, N 7.50. Found: C 68.58, H 5.89, N 7.17.

1. filtrationfiltered under nitrogen through a stainless steel
2. filtrationfilter
3. washThe filter cake was washed three times with ethyl acetate (30 mL)
4. customdried under a nitrogen
5. custompurge for 2 hours
6. customThe filter cake was then dried in a vacuum oven at 60° C. overnight