Reaktion #65184

Reaktionsgleichung

α-chloro-N,N-dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride

Rongalite

→

white solid

Ausbeute 71.7%

N,N-Dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]-benzothiazole-3-acetamide

Ausbeute 71.7%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe suspension is filtered
2. 2
   Waschenit is rinsed with dichloromethane
3. 3
   Waschenthe organic phase is washed (pH=1) with 500 ml of 0.5N sodium hydroxide up to a pH>10
4. 4
   TrocknenThe organic phase is dried over sodium sulphate
5. 5
   Sonstigethe solvent is evaporated under reduced pressure
6. 6
   SonstigeA beige-coloured solid is obtained which
7. 7
   Sonstigeis purified by chromatography on a silica gel column
8. 8
   Wascheneluting with a 95/5 mixture of dichloromethane/methanol

Vorschrift

40 g (0.0938 mole) of α-chloro-N,N-dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 1200 ml of dichloromethane are treated with 43.6 (0.283 mole) of Rongalite®, while stirring the mixture at room temperature for 6 h. The suspension is filtered, it is rinsed with dichloromethane and the organic phase is washed (pH=1) with 500 ml of 0.5N sodium hydroxide up to a pH>10, then to neutral pH with a saturated sodium chloride solution. The organic phase is dried over sodium sulphate and the solvent is evaporated under reduced pressure. A beige-coloured solid is obtained which is purified by chromatography on a silica gel column, eluting with a 95/5 mixture of dichloromethane/methanol. 23.9 g of a white solid are obtained. Melting point: 216°-218° C.

Quelle