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Hydrazine hydrate (1:1) → HCID 178509230, Verbindung

HRID 510027
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 510027
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]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 231108512-Chloro-5-fluoropyridine-3-carbonitrile

Produkt 1

HCID 178509230HCID 178509230, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 174Ethylene GlycolLösungsmittel

Versuchsvorschrift

A suspension of 38.5 g (245.93 mmol) of 2-chloro-5-fluoronicotinonitrile was initially charged in 1,2-ethanediol (380 ml), and hydrazine hydrate (119.6 ml, 2.459 mol) was then added. The mixture was heated under reflux while stirring for 4 h. The product precipitated out in the course of cooling. Water (380 ml) was added to the yellow crystals, and extraction was effected by stirring at RT for 10 min. The suspension was then filtered with suction through a frit and washed through with water (200 ml) and with THF at −10° C. (200 ml). The residue was dried under high vacuum over phosphorus pentoxide.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux
  3. customThe product precipitated out in the course
  4. temperatureof cooling
  5. additionWater (380 ml) was added to the yellow crystals, and extraction
  6. stirringby stirring at RT for 10 min
  7. filtrationThe suspension was then filtered with suction through a frit
  8. washwashed through with water (200 ml) and with THF at −10° C. (200 ml)
  9. dry with materialThe residue was dried under high vacuum over phosphorus pentoxide

Quellen und Nachweise

ORD-Eintrag
ord-95c48b4bbeba4e2bb24d034a4279465a
Quelldatensatz
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09096592B2

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