Reaktion #320067

Reaktionsgleichung

trifluoroacetic acid

2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-8-(2-acetylethyl)-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine

acetic acid

→

title compound

Ausbeute 65.8%

2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-11-hydroxy-8-(2-acetylethyl)-6,11-dihydrodibenz[b,e]oxepine

Ausbeute 65.8%

Lösungsmittel

dioxane

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeobtained in Reference example 74
2. 2
   workup.STIRRINGthe mixture was stirred for 10 hours
3. 3
   Sonstigewere removed by filtration
4. 4
   workup.DISSOLUTIONThe residue was dissolved in chloroform
5. 5
   Waschenthe organic layer was washed with water
6. 6
   Trocknendried over anhydrous sodium sulfate
7. 7
   SonstigeAfter the solvent was removed
8. 8
   Waschenthe residue was washed with a mixed solution of acetone and ether

Vorschrift

0.02 ml of trifluoroacetic acid was added to 0.73 g of 2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-8-(2-acetylethyl)-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine obtained in Reference example 74 dissolved in a mixed solution of 5 ml of dioxane and 2 ml of water, the mixture was stirred at room temperature for 15 minutes, 4 ml of acetic acid was added to the mixture and the mixture was stirred for 10 hours. 80 ml of water was added to the reaction mixture and insolubles were removed by filtration. The residue was dissolved in chloroform and the organic layer was washed with water and dried over anhydrous sodium sulfate. After the solvent was removed, the residue was washed with a mixed solution of acetone and ether to obtain 0.41 g of the title compound.

Quelle