Lithium borohydride → HCID 18779681, Verbindung

HRID 1585935Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1585935
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[N:11])=[C:6]([C:12]#[N:13])[CH:5]=1.[Li+].[BH4-]>C1COCC1>[OH:2][CH2:3][C:4]1[CH:5]=[C:6]([C:12]#[N:13])[C:7](=[CH:8][CH:9]=1)[C:10]#[N:11]

Komponenten

4

Edukt 2

HCID 4148881Lithium borohydrideHCID 14495336HCID 14495336, Verbindung

Produkt 1

HCID 18779681HCID 18779681, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

3,4-Dicyano-benzoic acid methyl ester from step 1 (2.4 g, 12.9 mmol ) was dissolved in THF (65 ml). LiBH4 in THF (2M, 12.9 ml, 25.8 mmol) was added. The reaction mixture was heated to 70° C. for 3 hours. The reaction was quenched carefully with 3N HCl and then extracted with EtOAc (3×20 mL). The organic layers were combined, washed with brine, dried (MgSO4), filtered and concentrated to yield the desired product. FAB MS: 159 m/z (M+ +H)

Aufarbeitung

  1. customThe reaction was quenched carefully with 3N HCl
  2. extractionextracted with EtOAc (3×20 mL)
  3. washwashed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-0afeabbe91bc4dc6bb161aec55760a0c
Quelldatensatz
uspto-grants-1999_08
Patentnummer
US05939439

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