Trimethyltin chloride → 5-Methyl-2-trimethylstannylbenzo[b]thiophene

HRID 53826

Reaktionsgleichung

Reaktionsgleichung von HRID 53826
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH:3]=1.C([Li])CCC.[CH3:16][Sn:17](Cl)([CH3:19])[CH3:18].[Cl-].[NH4+]>CCOCC.CCCCCC>[CH3:1][C:2]1[CH:10]=[CH:9][C:5]2[S:6][C:7]([Sn:17]([CH3:19])([CH3:18])[CH3:16])=[CH:8][C:4]=2[CH:3]=1

Komponenten

7

Edukt 4

HCID 14016Trimethyltin chlorideHCID 25517Ammonium ChlorideHCID 843465-Methylbenzo(b)thiopheneHCID 178418339Butyllithium

Produkt 1

HCID 218481335-Methyl-2-trimethylstannylbenzo[b]thiophene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittel3×HCID 8058HexaneLösungsmittel

Versuchsvorschrift

A solution of 7.411 g of 5-methylbenzo[b]thiophene (Maybridge, Chemical Co. Ltd., 11-78) in 35 ml of ether is added dropwise at 0° to a mixture of 40 ml of 1.5N butyllithium in hexane and 40 ml of ether. After 30 minutes, a solution of 9.963 g of trimethyltin chloride in 50 ml of ether is also added dropwise at 0°. After stirring for 1 hour at 0°, 50 ml of 5% ammonium chloride solution are added. The product is obtained by extracting with 100 ml and 150 ml of ether. Distillation at 0.15 mbar and 100°-106° yields 5-methyl-2-trimethylstannylbenzo[b]thiophene.

Aufarbeitung

  1. customThe product is obtained
  2. extractionby extracting with 100 ml and 150 ml of ether
  3. distillationDistillation at 0.15 mbar and 100°-106°

Quellen und Nachweise

ORD-Eintrag
ord-aac6fa2d8f224448bf2aa8d745c21d9b
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05620998

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