Tributylstannane → HCID 20061023, Verbindung

HRID 1085149Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1085149
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([C:13]#[N:14])=[CH:9][CH:8]=2)[C:5]([CH3:15])=[N:4][C:3]=1I.C([SnH](CCCC)CCCC)CCC.[F-].[K+].C1C[O:35][CH2:34]C1>>[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([C:13]#[N:14])=[CH:9][CH:8]=2)[C:5]([CH3:15])=[N:4][C:3]=1[CH:34]=[O:35]

Komponenten

5

Edukt 4

HCID 5948TributylstannaneHCID 8028Tetrahydrofuran2×HCID 522689Potassium FluorideHCID 20060989HCID 20060989, Verbindung

Produkt 1

HCID 20061023HCID 20061023, Verbindung

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A solution of the product from (b) (1.03 g, 3 mmol) and tetrakis (triphenylphosphine)palladium (0.3 g) in THF (70 ml) was installed under an atmosphere of carbon monoxide and heated to 50° C. Tributyltin hydride (0.96 g, 3.3 mmol) in THF (40 ml) was instilled by motor-driven syringe over 4.5 hours. After an additional 0.5 hours the mixture was stirred with 100 ml of 10% potassium fluoride solution for 15 minutes, then extracted twice with dichloromethane. The organic layers were dried over magnesium sulphate and evaporated to an orange solid.

Aufarbeitung

  1. extractionextracted twice with dichloromethane
  2. dry with materialThe organic layers were dried over magnesium sulphate
  3. customevaporated to an orange solid

Quellen und Nachweise

ORD-Eintrag
ord-8515b0802c154cb3bfff6ca4b2bbdeb1
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05008263

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