反应详情

A solution of the phthalimide VIII (4.9 g, 8.7 mmol) in ethanol (110 mL) containing hydrazine hydrate (75%, 1.48 mL) was heated at reflux for 6 hours. The ethanol was removed under reduced pressure and the residue was shaken with ether and 10% aqueous potassium hydroxide. The ether layer was washed with water (×2) and dried (K2CO3). To the dried ether solution of 1 as the free base, was added a solution of succinic acid (1.03 g, 1 mol equiv) in ether (100 mL) containing methanol (4 mL) to solubilize the succinic acid. After standing overnight, the solid was filtered to yield 4.5 g (94%) of the target compound (1), mp 102°-103° (eff).

1. temperaturewas heated
2. temperatureat reflux for 6 hours
3. customThe ethanol was removed under reduced pressure
4. washThe ether layer was washed with water (×2)
5. dry with materialdried (K2CO3)
6. filtrationthe solid was filtered