Hydrochloric Acid → HCID 15137264, Verbindung

HRID 1741560Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1741560
C[O:2][C:3]([C:5]1[CH:10]=[C:9]([C:11]2[CH:16]=[C:15]([C:17](OC)=[O:18])[N:14]=[C:13]([C:21](OC)=[O:22])[CH:12]=2)[CH:8]=[C:7]([C:25](OC)=[O:26])[N:6]=1)=O.[BH4-].[Na+].Cl>O1CCOCC1.O>[OH:18][CH2:17][C:15]1[CH:16]=[C:11]([C:9]2[CH:10]=[C:5]([CH2:3][OH:2])[N:6]=[C:7]([CH2:25][OH:26])[CH:8]=2)[CH:12]=[C:13]([CH2:21][OH:22])[N:14]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 2762456Tetramethyl [4,4'-bipyridine]-2,2',6,6'-tetracarboxylateHCID 4311764Sodium borohydride

Produkt 1

HCID 15137264HCID 15137264, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

50 g (128.77 mmol) of 2,2', 6,6'-tetra(methoxycarbonyl)-4,4'-bipyridine is dissolved in a mixture of 400 ml of dioxane/400 ml of water and, in portions, 48.71 g (1.28 mol) of sodium borohydride is added thereto. The mixture is stirred overnight at room temperature. The solution is acidified with 5N hydrochloric acid and evaporated to dryness. The residue is suspended in 1 liter of 1N sodium hydroxide solution and extracted three times with 250 ml of chloroform. The organic phases are dried over magnesium sulfate and evaporated under vacuum. The residue is recrystallized from ethanol/ether.

Aufarbeitung

  1. additionis added
  2. customevaporated to dryness
  3. extractionextracted three times with 250 ml of chloroform
  4. dry with materialThe organic phases are dried over magnesium sulfate
  5. customevaporated under vacuum
  6. customThe residue is recrystallized from ethanol/ether

Quellen und Nachweise

ORD-Eintrag
ord-8cb5219b9d394ea4b007966a524147c7
Quelldatensatz
uspto-grants-1994_08
Patentnummer
US05334371

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