Hydrochloric Acid → HCID 22717665, Verbindung

HRID 1582543Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1582543
[NH2:1][C:2]1[S:3][C:4]([I:11])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.[S:12]1[CH:16]=[CH:15][CH:14]=[C:13]1[C:17](Cl)=[O:18].Cl>N1C=CC=CC=1>[I:11][C:4]1[S:3][C:2]([NH:1][C:17]([C:13]2[S:12][CH:16]=[CH:15][CH:14]=2)=[O:18])=[N:6][C:5]=1[C:7]([F:10])([F:8])[F:9]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 789282-Thiophenecarbonyl chlorideHCID 227176715-Iodo-4-(trifluoromethyl)-1,3-thiazol-2-amine

Produkt 1

HCID 22717665HCID 22717665, VerbindungAusbeute 72,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

2-Amino-5-iodo-4-trifluoromethylthiazole (1.2 g) was dissolved in pyridine (2 ml) and thiophene-2-carbonyl chloride (0.80 g) was added at room temperature with stirring. The mixture was stirred for 6 hr at room temperature. The mixture was poured into ice water and acidified with aqueous hydrochloric acid then extracted with chloroform The chloroform layer was dried over magnesium sulfate and the solvent was removed under reduced pressure. The solid thus obtained was recrystallized from methanol to give N-(5-iodo-4-trifluoromethylthiazol-2-yl)thiophene-2-carboxamide (1.2 g), m. p. 184-185° C.

Aufarbeitung

  1. stirringThe mixture was stirred for 6 hr at room temperature
  2. extractionthen extracted with chloroform The chloroform layer
  3. dry with materialwas dried over magnesium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe solid thus obtained
  6. customwas recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-b05070522deb41ff9b3b82e2ffab796f
Quelldatensatz
uspto-grants-2004_05
Patentnummer
US06737382B1

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