Reaktion #75000
ord-190279ac6ac94ac49644cabe172141dd
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturchilled (0°) solution
- 2workup.STIRRINGThe reaction mixture was stirred at ambient temperature for 1 hour
- 3Einengenconcentrated to dryness under reduced pressure
- 4workup.ADDITIONThe residue was treated with water
- 5Filtrationfiltered
- 6Sonstigerecrystallized from ethanol
Vorschrift
To a stirred and chilled (0°) solution containing 200 g (0.86 mol) of 2-bromo-4-nitrophenylhydrazine (m.p. 143°-145°) and 116.8 g (0.9 mol) of ethyldiisopropylamine in 1000 ml of tetrahydrofuran was added dropwise 108.5 g (0.9 mol) of pivaloyl chloride. The reaction mixture was stirred at ambient temperature for 1 hour and then concentrated to dryness under reduced pressure. The residue was treated with water, filtered and recrystallized from ethanol to give 165 g (52%) of product as a light yellow solid; m.p. 145° C.