Reaktion #998524

Reaktionsgleichung

copper(I) cyanide

6-bromobenzo[b]thiophene

ethylenediamine

→

desired intermediate

Ausbeute 78.0%

Benzo[b]thiophen-6-carbonitrile

Ausbeute 78.0%

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   WaschenWash the organic mixture with brine
2. 2
   Trocknendry over Na2SO4
3. 3
   Sonstigeevaporate
4. 4
   SonstigePurify by chromatography on silica gel eluting with EtOAc/hexane (0:1 to 1:3)

Vorschrift

Heat copper(I) cyanide (0.84 g, 9.4 mmol) and 6-bromobenzo[b]thiophene (prepared as described in WO 01/23381) (1.0 g, 4.7 mmol) at 160° C. for 13 h. Cool the mixture to 0° C., add 33% aqueous ethylenediamine (20 mL) and dilute with ether. Wash the organic mixture with brine, dry over Na2SO4 and evaporate. Purify by chromatography on silica gel eluting with EtOAc/hexane (0:1 to 1:3) to give the desired intermediate (0.58 g, 78%). GC-MS m/z: 159 (M+).

Quelle