Water → 10,11-Dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin-10-ol

HRID 435658Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 435658
[F:1][C:2]([F:20])([F:19])[C:3]1[CH:18]=[CH:17][C:6]2[S:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[C:10](=[O:12])[CH2:11][C:5]=2[CH:4]=1.[BH4-].[Na+].O.C(Cl)(Cl)Cl>C(O)C>[F:20][C:2]([F:1])([F:19])[C:3]1[CH:18]=[CH:17][C:6]2[S:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[CH:10]([OH:12])[CH2:11][C:5]=2[CH:4]=1

Komponenten

6

Reaktionsbedingungen

Temperatur
30 °C

Versuchsvorschrift

12 g of 10,11-dihydro-2-trifluoromethyl-dibenzo[b,f]-thiepin-10-one are dissolved in 110 ml of absolute ethanol and treated with 4 g of sodium borohydride. The mixture is held at reflux for 12 minutes, cooled to 30° C and treated with 350 ml of water and 100 ml of chloroform. After equilibration, the organic phase is washed with aqueous sodium chloride solution, dried over sodium sulphate and evaporated under reduced pressure. There is obtained 10,11-dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin-10-ol in the form of yellow crystals which melt at 122°-123° C.

Aufarbeitung

  1. temperatureat reflux for 12 minutes
  2. washAfter equilibration, the organic phase is washed with aqueous sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b580036d12424d9a9647f84b78065018
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04006145

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