Lithium borohydride → HCID 18779681, Verbindung

HRID 1421762Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1421762
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 (2 M, 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.

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-d0684c9bc57c46819bd5b608c81902ac
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06077853

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