Reaktion #1848984

Reaktionsgleichung

(5-chlorothien-2-yl)methoxyamine

2-acetyl-3-acetyloxy-5-(tetrahydro-2H-thiopyran-3-yl)cyclohex-2-en-1-one

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title compound

3-Acetyloxy-2-[1-[(5-chlorothien-2-yl)methoxyimino]ethyl]-5-(tetrahydro-2H-thiopyran-3-yl)-cyclohex-2-en-1-one

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction mixture is concentrated under reduced pressure
2. 2
   workup.ADDITIONThe resulting residue is diluted with 25 ml of dichloromethane
3. 3
   Waschenwashed twice with 10 ml of saturated sodium chloride solution
4. 4
   ExtraktionThe washed extract
5. 5
   Trocknenis then dried over anhydrous magnesium sulfate
6. 6
   Sonstigeevaporated under reduced pressure
7. 7
   SonstigeThe product can then be purified by column chromatography

Vorschrift

0.34 g (2.0 mmol) of (5-chlorothien-2-yl)methoxyamine is added to a stirred solution of 0.59 g (2.0 mmol) of 2-acetyl-3-acetyloxy-5-(tetrahydro-2H-thiopyran-3-yl)cyclohex-2-en-1-one in 10 ml of absolute ethanol. After stirring overnight at room temperature, the reaction mixture is concentrated under reduced pressure. The resulting residue is diluted with 25 ml of dichloromethane and washed twice with 10 ml of saturated sodium chloride solution. The washed extract is then dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The product can then be purified by column chromatography employing tetrahydrofuran-hexane (1:2 by volume) as eluent to afford the title compound.

Quelle