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Sodium Methoxide → HCID 15008938, Verbindung

HRID 654268
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 654268
[CH3:1][O-:2].[Na+].[CH3:4][NH:5][C:6]1[N:11]=[C:10](C(Cl)(Cl)Cl)[N:9]=[C:8]([C:16]([F:19])([F:18])[F:17])[N:7]=1>CO.O.Cl>[CH3:1][O:2][C:10]1[N:11]=[C:6]([NH:5][CH3:4])[N:7]=[C:8]([C:16]([F:19])([F:18])[F:17])[N:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 10942334Sodium Methoxide2×HCID 15008937N-Methyl-4-(trichloromethyl)-6-(trifluoromethyl)-1,3,5-triazin-2-amine

Produkt 1

HCID 15008938HCID 15008938, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313Hydrochloric AcidLösungsmittelHCID 887MethanolLösungsmittel3×
HCID 962
Water
Lösungsmittel

Versuchsvorschrift

21.8 g of a 30% strength solution of sodium methanolate in methanol (0.12 mol of sodium methanolate) were added dropwise to a solution of 119.4 g (0.40 mol) of 2-methylamino-4-trichloromethyl-6-trifluoromethyl-1,3,5-triazine in 400 ml of methanol. The resulting yellow mixture was then refluxed for 1 hour during which it gradually became cloudy. After addition of a further 7.2 g of the 30% strength solution of sodium methanolate in methanol (0.04 mol of sodium methanolate), the mixture was refluxed for a further 30 minutes and, after cooling to 20° to 25° C., diluted with 150 ml of water and neutralized with 1 normal aqueous hydrochloric acid. The solvent was then removed at 40° C. under reduced pressure, after which the resulting solid was separated off and dried at 40° C. under reduced pressure for 15 hours.

Aufarbeitung

  1. temperatureThe resulting yellow mixture was then refluxed for 1 hour during which it gradually became cloudy
  2. temperaturethe mixture was refluxed for a further 30 minutes
  3. temperatureafter cooling to 20° to 25° C.
  4. customThe solvent was then removed at 40° C. under reduced pressure
  5. customafter which the resulting solid was separated off
  6. customdried at 40° C. under reduced pressure for 15 hours

Quellen und Nachweise

ORD-Eintrag
ord-412da58d239e4001a5a6c6a8595d92ff
Quelldatensatz
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05130428

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