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Ammonia → 2,2-Difluoro-2-phenylacetamide

HRID 1457209
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1457209
[F:1][C:2]([F:14])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:3](OCC)=[O:4].[NH3:15]>CCO>[F:1][C:2]([F:14])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:3]([NH2:15])=[O:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 10631860Ethyl 2,2-difluoro-2-phenylacetate

Produkt 1

HCID 2696562,2-Difluoro-2-phenylacetamideAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of the title compound of Step (A) (6.00 g; 30 mmol) in 50 ml of EtOH was saturated with anhydrous NH3. An exothermic reaction was observed. After stirring the reaction mixture 60 hr at room temperature, the volatiles were removed in vacuo and the solid residue was taken up in a minimal amount of hot ethyl acetate. A small amount of insoluble material was filtered off and hexane was added to the filtrate until slightly turbid. After cooling to room temperature and standing several hr, the crystals were filtered and dried to afford 4.68 g (91%) of the title compound of this step as a colorless crystalline solid.

Aufarbeitung

  1. customAn exothermic reaction
  2. customthe volatiles were removed in vacuo
  3. filtrationA small amount of insoluble material was filtered off
  4. additionhexane was added to the filtrate until slightly turbid
  5. temperatureAfter cooling to room temperature
  6. waitstanding several hr
  7. filtrationthe crystals were filtered
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f969fd42a4e149a1a52bb36191ea5073
Quelldatensatz
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05846990

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