Hydrazine hydrate (1:1) → HCID 178509230, Verbindung
Reaktionsgleichung
Cl[C:2]1[N:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[C:4]#[N:5].O.[NH2:12][NH2:13]>C(O)CO>[F:10][C:7]1[CH:6]=[C:3]2[C:4]([NH2:5])=[N:13][NH:12][C:2]2=[N:9][CH:8]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A suspension of 38.5 g (245.93 mmol) of 2-chloro-5-fluoronicotinonitrile in 1,2-ethanediol (380 ml) was prepared and then hydrazine hydrate (119.6 ml) was added. It was heated under reflux for 4 h, with stirring. On cooling, the product was precipitated. Water (380 ml) was added to the crystals and it was left to precipitate for 10 min at RT. Then the suspension was filtered with suction on a frit, and washed again with water (200 ml) and with cold (−10° C.) THF (200 ml). Drying over phosphorus pentoxide under high vacuum.
Aufarbeitung
- customwas prepared
- temperatureIt was heated
- temperatureunder reflux for 4 h
- temperatureOn cooling
- customthe product was precipitated
- additionWater (380 ml) was added to the crystals and it
- waitwas left
- customto precipitate for 10 min at RT
- filtrationThen the suspension was filtered with suction on a frit
- washwashed again with water (200 ml) and with cold (−10° C.) THF (200 ml)
- dry with materialDrying over phosphorus pentoxide under high vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-abde68c3ca77470c9033206fa70d51ac
- Quelldatensatz
- uspto-grants-2014_10
- Patentnummer
- US08859569B2
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