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Acetone → HCID 19417509, Verbindung

HRID 864965
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 864965
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][C:9]=1[O:10][CH3:11])[NH2:6].[C:12]([NH:14][C:15]([NH2:17])=[NH:16])#[N:13].[CH3:18][C:19]([CH3:21])=O>>[ClH:2].[Cl:2][C:3]1[CH:4]=[C:5]([N:6]2[C:19]([CH3:21])([CH3:18])[N:16]=[C:15]([NH2:17])[N:14]=[C:12]2[NH2:13])[CH:7]=[CH:8][C:9]=1[O:10][CH3:11]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 180AcetoneHCID 122278893-Chloro-4-methoxyaniline hydrochlorideHCID 178418324HCID 178418324, Verbindung

Produkt 1

HCID 19417509HCID 19417509, Verbindung

Versuchsvorschrift

A stirred mixture of 3.0 grams (0.019 mole) of 90% pure 3-chloro-4-methoxyaniline and 4 mL of concentrated hydrochloric acid in 20 mL of toluene was heated to reflux using a heat gun. The reaction mixture was then concentrated under reduced pressure to a residue. The residue was triturated with 50 mL of diethyl ether, and the resultant solid was collected by filtration. The solid was dried under vacuum, yielding 3.4 grams (0.018 mole) of 3-chloro-4-methoxyaniline hydrochloride. A stirred mixture of the aniline hydrochloride and 1.8 grams (0.022 mole) of cyanoguanidine in 25 mL of acetone was then heated at reflux for about 20 hours. The mixture was cooled, and a solid was collected by filtration. The solid was dried under vacuum, yielding 4.9 grams of 1-(3-chloro-4-methoxyphenyl)-2,4-diamino-6,6-dimethyl-1,6-dihydro-1,3,5-triazine hydrochloride, mp 232 ° C. The NMR spectrum was consistent with the proposed structure.

Aufarbeitung

  1. temperaturewas then heated
  2. temperatureat reflux for about 20 hours
  3. temperatureThe mixture was cooled
  4. filtrationa solid was collected by filtration
  5. customThe solid was dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-4de5d58509204282b1b09c6e4b06bc5e
Quelldatensatz
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05565451

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