Diphosgene → HCID 10998791, Verbindung

HRID 846291Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 846291
[F:1][C:2]([F:13])([F:12])[C:3]1[S:4][C:5]([C:9](O)=[O:10])=[C:6]([CH3:8])[N:7]=1.[Cl:14]C(OC(Cl)(Cl)Cl)=O>ClC1C=CC=CC=1.N1C=CC=CC=1>[F:1][C:2]([F:13])([F:12])[C:3]1[S:4][C:5]([C:9]([Cl:14])=[O:10])=[C:6]([CH3:8])[N:7]=1

Komponenten

5

Edukt 2

HCID 10426DiphosgeneHCID 108999004-Methyl-2-(trifluoromethyl)-1,3-thiazole-5-carboxylic acid

Produkt 1

HCID 10998791HCID 10998791, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineKatalysatorHCID 7964ChlorobenzeneLösungsmittel

Versuchsvorschrift

In a similar apparatus to Example 1, 4.2 g (0.02 mole) of 2-trifluoromethyl-4-methylthiazole-5-carboxylic acid were suspended in 100 ml of chlorobenzene, followed by the addition of 0.04 g of pyridine. Under heating and reflux, 9.9 g (0.05 mole) of trichloromethyl chloroformate were added dropwise over 5 hours. After completion of the dropwise addition, stirring was continued for additional 2 hours. After completion of the reaction, the reaction mixture was filtered and the filtrate was concentrated to obtain 4.5 g of 2-trifluoromethyl-4-methylthiazole-5-carboxylic acid chloride. Its purity and yield were 98.7% and 98.0%, respectively.

Aufarbeitung

  1. temperatureUnder heating
  2. temperaturereflux
  3. additionAfter completion of the dropwise addition
  4. customAfter completion of the reaction
  5. filtrationthe reaction mixture was filtered
  6. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-2bdc6714dcb7439ba6c6637e0ccccbfb
Quelldatensatz
uspto-grants-1992_08
Patentnummer
US05136042

Notizen zur Reaktion

Wird geladen…