Reaktion #63813

Reaktionsgleichung

6(1,1-dimethylethyl)-3-hydroxy-2-phenyl-7-azabenzo[b]thiophene

sodium acetate

→

fine white needles

Ausbeute 91.6%

3-Acetoxy-6-(1,1-dimethylethyl)-2-phenyl-7-azabenzo[b]thiophene

Ausbeute 91.6%

Lösungsmittel

acetic anhydride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 1 hour
2. 2
   EinengenThe solution was concentrated
3. 3
   Sonstigethe residue was partitioned between ether and water
4. 4
   WaschenThe ether layer was washed with sodium bicarbonate solution and brine
5. 5
   Sonstigedried
6. 6
   Einengenconcentrated
7. 7
   SonstigeThe residue was crystallized from ether-hexane

Vorschrift

A solution of 1.42 g (5 mmol) of 6(1,1-dimethylethyl)-3-hydroxy-2-phenyl-7-azabenzo[b]thiophene and 1.42 g sodium acetate in 20 mL of acetic anhydride was heated at reflux for 1 hour. The solution was concentrated and the residue was partitioned between ether and water. The ether layer was washed with sodium bicarbonate solution and brine, dried and concentrated. The residue was crystallized from ether-hexane to afford 1.49 g (91%) of fine white needles, m.p. 128°-9° C.

Quelle