反应详情

A suspension of 2-tert-butyl-5-chloro-3-hydroxyisoindolin-1-one (5.26 g, 21.9 mmol) in glacial acetic acid (32 mL) was heated with stirring until the mixture became a clear solution. Anhydrous hydrazine (1.0 mL, 22 mmol) was added dropwise and the resultant solution was stirred at reflux overnight. The reaction mixture was concentrated under reduced pressure. Water was added to the mixture, after which a solid material precipitated out of the solution. The solid was collected by filtration and rinsed thoroughly with water, followed by air-drying to afford 6-chlorophthalazin-1-ol (3.9 g, 98% yield) as an off-white powder (mp 271-273° C.).

1. temperaturewas heated
2. temperatureat reflux overnight
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additionWater was added to the mixture
5. customafter which a solid material precipitated out of the solution
6. filtrationThe solid was collected by filtration
7. washrinsed thoroughly with water
8. customby air-drying