Reaktion #495809

Reaktionsgleichung

oxalyl chloride

benzothiophene carboxylic acid

DMF

→

benzo[b]thiophene-3-carbonyl chloride

Lösungsmittel

MeTHF

MeTHF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction mixture is concentrated to 5 volumes
2. 2
   Sonstigeto remove the excess of oxalyl chloride

Vorschrift

To benzothiophene carboxylic acid (7 g) in MeTHF (6.5 Vols, 45.5 mL) is added a catalytic amount of DMF (0.01 eq.). Then, oxalyl chloride (1.1 eq.) is charged slowly to control the gaz release. After 16 h of stirring at 20° C., the end of the reaction is controlled by HPLC. MeTHF (6.5 Vols) is next added and the reaction mixture is concentrated to 5 volumes to remove the excess of oxalyl chloride. The resulting benzo[b]thiophene-3-carbonyl chloride is stored in a MeTHF solution.

Quelle