Water → HCID 5282563, Verbindung

HRID 379580Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 379580
[BH4-].[Na+].[NH2:3][C:4]1[S:5][CH:6]=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].O.C(=O)(O)[O-].[Na+]>C(O)(=O)C(C)C>[CH3:6][CH:7]([CH3:14])[CH2:8][NH:3][C:4]1[S:5][CH:6]=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

Komponenten

6

Edukt 4

HCID 962WaterHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydride2×HCID 52825623,4-Diethyl 2-aMinothiophene-3,4-dicarboxylate

Produkt 1

HCID 5282563HCID 5282563, VerbindungAusbeute 172,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6590Isobutyric AcidLösungsmittel

Versuchsvorschrift

Sodium borohydride (18 g) was added portionwise over 5 hours to a stirred suspension of diethyl 2-aminothiophene-3,4-dicarboxyate (33 g) in isobutyric acid (300 ml) at room temperature. The mixture was stirred for 16 hours then further sodium borohydride (4 g) was added and stirring was continued for 5 hours. Water (1.51) was added, the mixture was neutralised by addition of solid sodium bicarbonate and then extracted with ether (3×500 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated to give the subtitle compound (35 g) as a solid.

Aufarbeitung

  1. stirringstirring
  2. waitwas continued for 5 hours
  3. extractionextracted with ether (3×500 ml)
  4. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-95cb73f5693144e38dd0ae18fd3a6c07
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06300334B1

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