Reaktion #348742

Reaktionsgleichung

2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-one

sodium boron hydride

→

2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling over a period of 5 minutes
2. 2
   Sonstigethe mixture was reacted at room temperature for 30 minutes
3. 3
   Temperaturrefluxed for 15 minutes
4. 4
   workup.DISTILLATIONwas distilled off
5. 5
   TemperaturAfter cooling, to the mixture
6. 6
   workup.ADDITIONwas added water
7. 7
   Extraktionthe mixture was extracted with chloroform
8. 8
   WaschenThe extract was washed with water
9. 9
   Trocknendried over anhydrous sodium sulfate

Vorschrift

To the mixture of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-one obtained in Example 40 and 10 ml of methanol was gradually added 0.2 g of sodium boron hydride with ice-cooling over a period of 5 minutes and the mixture was reacted at room temperature for 30 minutes and refluxed for 15 minutes. After the completion of the reaction, methanol was distilled off. After cooling, to the mixture was added water and the mixture was extracted with chloroform. The extract was washed with water, dried over anhydrous sodium sulfate and freed of the solvent to obtain 0.5 g of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol as colorless crystals having a melting point of 130°-132° C.

Quelle