Ammonia → 3-Phenyl-6-pyridazone

Temperatur

40 °C

19.6 g (162.95 mmol) of 1-phenylethanone and 5 g (54.32 mmol) of oxoacetate monohydrate were stirred at 100° C. for 2 hours. The reaction solution was then cooled to 40° C., and 20 ml of water and 4 ml of ammonia were added. The mixture was then twice extracted with 50 ml of dichloromethane. 2.64 ml (53.32 mmol) of hydrazine monohydrate were then added to the aqueous phase obtained, and the mixture was stirred at 100° C. for 2 hours. After the reaction, the reaction solution was cooled to room temperature. The precipitated crystals were filtered off with suction, washed with water and dried in a vacuum drying cabinet at 50° C. overnight. This gave 4.3 g (24.97 mmol, 15% of theory) of the title compound as colorless crystals.

1. extractionThe mixture was then twice extracted with 50 ml of dichloromethane
2. customobtained
3. customAfter the reaction
4. temperaturethe reaction solution was cooled to room temperature
5. filtrationThe precipitated crystals were filtered off with suction
6. washwashed with water
7. customdried in a vacuum
8. customdrying cabinet at 50° C. overnight

ORD-Eintrag

ord-7abf0e199c0a420bbf6b4612125e53d1

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08987256B2