Reaktion #65461

Reaktionsgleichung

compound

6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin

acetic anhydride

sodium hydrogen carbonate

→

6-Acetoxy-2-{4-[bis(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin

Ausbeute 92.0%

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionAfter extraction with ether (2×25 ml)
2. 2
   Sonstigethe product is purified by chromatography on a silica column (eluant:ethyl acetate/petroleum ether, 20:80)
3. 3
   Sonstigeobtained in pure form as a solid in a yield of 92%

Vorschrift

Dissolve 0.5 g (1.07 mmol) of the compound obtained in Example 1 at 0° C. in 0.255 ml (2.7 mmol) of acetic anhydride under an inert atmosphere. Add 2 volumes of pyridine (0.5 10 ml) and continue stirring while returning to room temperature for a period of 1 h 30. Neutralise with a saturated sodium hydrogen carbonate solution. After extraction with ether (2×25 ml), the product is purified by chromatography on a silica column (eluant:ethyl acetate/petroleum ether, 20:80) and obtained in pure form as a solid in a yield of 92%.

Quelle