Reacción #348742

Ecuación de reacción

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

Disolventes

methanol

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturacooling over a period of 5 minutes
2. 2
   Otrothe mixture was reacted at room temperature for 30 minutes
3. 3
   Temperaturarefluxed for 15 minutes
4. 4
   workup.DISTILLATIONwas distilled off
5. 5
   TemperaturaAfter cooling, to the mixture
6. 6
   workup.ADDITIONwas added water
7. 7
   Extracciónthe mixture was extracted with chloroform
8. 8
   LavadoThe extract was washed with water
9. 9
   Secadodried over anhydrous sodium sulfate

Procedimiento

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.

Fuente