Pentafluoropropionic acid → HCID 178499322, Verbindung

HRID 2211294

Reaktionsgleichung

Reaktionsgleichung von HRID 2211294
[NH2:1][C:2]1[C:6]([NH2:7])=[C:5]([CH3:8])[S:4][C:3]=1[C:9]([O:11][CH3:12])=[O:10].[F:13][C:14]([F:22])([F:21])[C:15]([F:20])([F:19])[C:16](O)=O>>[CH3:8][C:5]1[S:4][C:3]([C:9]([O:11][CH3:12])=[O:10])=[C:2]2[C:6]=1[NH:7][C:16]([C:15]([F:20])([F:19])[C:14]([F:22])([F:21])[F:13])=[N:1]2

Komponenten

3

Edukt 2

HCID 62356Pentafluoropropionic acidHCID 18693138Methyl 3,4-diamino-5-methylthiophene-2-carboxylate

Produkt 1

HCID 178499322HCID 178499322, Verbindung

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of methyl 3,4-diamino-5-methylthiophene-2-carboxylate (1.0 g) in pentafluoropropionic acid (8.9 g) was stirred at 100° C. for 6 hr. The reaction solution was concentrated to dryness and the residue was suspensed in water. The mixture was made basic with aqueous solution of K2CO3, followed by extraction with ethyl acetate. The organic layer was washed with water, dried and concentrated to dryness. The residue was purified by silica gel column chromatography to give crystals. Recrystallization from isopropyl ether-hexane gave colorless plates (0.86 g, 51%). m.p. 156°-157° C.

Aufarbeitung

  1. concentrationThe reaction solution was concentrated to dryness
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with water
  4. customdried
  5. concentrationconcentrated to dryness
  6. customThe residue was purified by silica gel column chromatography
  7. customto give crystals
  8. customRecrystallization from isopropyl ether-hexane
  9. customgave colorless plates (0.86 g, 51%)

Quellen und Nachweise

ORD-Eintrag
ord-0b542faa7968475393bf06b11052ba00
Quelldatensatz
uspto-grants-1995_10
Patentnummer
US05463073

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