Reaktion #346716

Reaktionsgleichung

compound

5,6-Dimethoxy-1,2-benzisothiazoline-3-one-1,1-dioxide

lithium aluminum hydride

lithium aluminum hydride

ethyl acetate

aluminum hydroxide

→

5,6-Dimethoxy-1,2-benzisothiazoline-1,1-dioxide

Lösungsmittel

water

hydrochloric acid

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   workup.DISSOLUTIONwas dissolved
3. 3
   ExtraktionThe reaction solution now extracted with ethyl acetate
4. 4
   Waschenthe organic phase was washed with water
5. 5
   Sonstigedried
6. 6
   Sonstigeevaporated in vacuo
7. 7
   Filtrationthe desired compound was suction-filtered off

Vorschrift

7 gm (288 millimols) of the compound obtained in step (c) were refluxed for 2 hours with 3.3 gm (865 millimols) of lithium aluminum hydride in 400 ml of tetrahydrofuran. After cooling, the excess lithium aluminum hydride was decomposed by addition of ethyl acetate, the mixture was diluted with water, and subsequently 2 N hydrochloric acid was added until the aluminum hydroxide precipitate was dissolved. The reaction solution now extracted with ethyl acetate, and the organic phase was washed with water, dried and evaporated in vacuo. The residue was digested in ether, and the desired compound was suction-filtered off.

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