Reaktion #1129188

Reaktionsgleichung

hydrazine hydrate

1,4-dichlorophthalazine

ammonium hydroxide

Hydrazine hydrate

→

11

Ausbeute 84.0%

1-Chloro-4-hydrazinylphthalazine

Ausbeute 84.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigea thick precipitate formed
2. 2
   workup.ADDITIONthe temperature was kept below 74° C. by controlled addition of reagent
3. 3
   workup.ADDITIONAfter the addition
4. 4
   Temperaturwas heated
5. 5
   Temperaturat reflux for 10 min
6. 6
   Temperaturto cool
7. 7
   FiltrationThe reaction was filtered
8. 8
   Waschenthe solids were washed with water (20 mL) and ethanol (20 mL)
9. 9
   Sonstigedried at 40° C. in a vacuum oven overnight
10. 10
    SonstigeThe crude material was recrystallized from acetonitrile

Vorschrift

A mixture of 1,4-dichlorophthalazine 23 (10.2 g, 51.2 mmol) and ammonium hydroxide (4.5 mL) in ethanol (110 mL) was heated to 60° C. Hydrazine hydrate (9 mL, 179 mmol) was added dropwise. After about one-half of the hydrazine hydrate was added, a thick precipitate formed. The mixture was stirred well and the temperature was kept below 74° C. by controlled addition of reagent. After the addition was complete the reaction was heated at reflux for 10 min, then allowed to cool. The reaction was filtered and the solids were washed with water (20 mL) and ethanol (20 mL), then dried at 40° C. in a vacuum oven overnight. The crude material was recrystallized from acetonitrile to afford 8.38 g (84%) of 11 as a yellow solid.

Quelle