反应详情

The ester of Example 4, Step B (0.5 g, 1.6 mmol), hydroxylamine hydrochloride (0.17 g, 2.4 mmol), and 25 ml pyridine were refluxed for 3.5 h. The reaction mixture was poured into water, extracted with CHCl3. The organic phase was then washed with 1.0N HCl, water, dilute NaHCO3, water, and brine, dried (MgSO4) and evaporated to yield a crude solid which was purified by filtration through a pad of silica gel and celite. The product, 0.33 g was isolated as a solid, m. p. 188°-190° C.

1. extractionextracted with CHCl3
2. washThe organic phase was then washed with 1.0N HCl, water, dilute NaHCO3, water, and brine
3. dry with materialdried (MgSO4)
4. customevaporated
5. customto yield a crude solid which
6. filtrationwas purified by filtration through a pad of silica gel and celite
7. customThe product, 0.33 g was isolated as a solid, m. p. 188°-190° C.