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Hydrochloric Acid → N1-(2,4-Difluorobenzyl)-3-Chloro-2,2-Dimethylpropanamide

HRID 974399
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 974399
[F:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5].N1C=CC=CC=1.[Cl:17][CH2:18][C:19]([CH3:24])([CH3:23])[C:20](Cl)=[O:21].Cl>C1(C)C=CC=CC=1>[Cl:17][CH2:18][C:19]([CH3:24])([CH3:23])[C:20]([NH:5][CH2:4][C:3]1[CH:6]=[CH:7][C:8]([F:10])=[CH:9][C:2]=1[F:1])=[O:21]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 613453-Chloro-2,2-dimethylpropanoyl chlorideHCID 27332442,4-Difluorobenzylamine

Produkt 1

HCID 2779689N1-(2,4-Difluorobenzyl)-3-Chloro-2,2-Dimethylpropanamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140
Toluene
Lösungsmittel

Versuchsvorschrift

28.6 g (0.20 mol) of 2,4-difluorobenzylamine and 19.0 g (0.24 mol) of pyridine are dissolved in 100 ml of toluene. 34.1 g (0.22 mol) of chloropivaloyl chloride are added dropwise to this solution at 20°-25° C. over the course of 15 minutes with ice-bath cooling. A suspension forms and is stirred for a further 3 hours at room temperature until the reaction is complete (GC check). For work-up, the pH is adjusted to between 1 and 2 using 50 ml of 2N hydrochloric acid. The white emulsion produced is extracted three times with 100 ml of toluene. The extract is washed with 100 ml of water, dried using magnesium sulfate and evaporated on a vacuum rotary evaporator. 49.2 g (94% of theory) of a yellow oil are obtained.

Aufarbeitung

  1. temperaturecooling
  2. customThe white emulsion produced
  3. extractionis extracted three times with 100 ml of toluene
  4. washThe extract is washed with 100 ml of water
  5. customdried
  6. customevaporated on a vacuum rotary evaporator
  7. custom49.2 g (94% of theory) of a yellow oil are obtained

Quellen und Nachweise

ORD-Eintrag
ord-fc63af1e980343348e0addb8c65b36a5
Quelldatensatz
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05068371

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