Réaction #348742

Équation de réaction

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

Solvants

methanol

methanol

Conditions de réaction

Traitement

1. 1
   Températurecooling over a period of 5 minutes
2. 2
   Autrethe mixture was reacted at room temperature for 30 minutes
3. 3
   Températurerefluxed for 15 minutes
4. 4
   workup.DISTILLATIONwas distilled off
5. 5
   TempératureAfter cooling, to the mixture
6. 6
   workup.ADDITIONwas added water
7. 7
   Extractionthe mixture was extracted with chloroform
8. 8
   LavageThe extract was washed with water
9. 9
   Séchagedried over anhydrous sodium sulfate

Mode opératoire

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.

Source