Hydracrylonitrile → 2-(7-Chloroquinolin-2-yl)methoxy-11-(2-cyanoethoxy)-6,11-dihydrodibenz[b,e]oxepine

Under ice cooling and stirring, 0.27 ml of thionyl chloride was added 1.5 g of 2-(7-chloroquinolin-2-yl)methoxy-11-hydroxy-6,11-dihydrodibenz[b,e]oxepine obtained in Reference example 36 suspended in 30 ml of methylene chloride and the mixture was stirred at the same temperature for 40 minutes. After completion of the reaction, the reaction mixture was condensed under reduced pressure, the residue was dissolved in 12 ml of methylene chloride, 0.81 ml of ethylenecyanhydrin and 0.94 ml of triethylamine were added to the solution under ice cooling and stirring and the mixture was stirred at room temperature for 2.5 hours. The reaction mixture was washed with water and the organic layer was dried over anhydrous sodium sulfate. Solid obtained by removing the solvent was washed with a diethyl ether-hexane mixed solution to obtain 1.31 g of the title compound.

1. customobtained in Reference example 36
2. stirringthe mixture was stirred at the same temperature for 40 minutes
3. customAfter completion of the reaction
4. customcondensed under reduced pressure
5. stirringstirring
6. stirringthe mixture was stirred at room temperature for 2.5 hours
7. washThe reaction mixture was washed with water
8. dry with materialthe organic layer was dried over anhydrous sodium sulfate
9. customSolid obtained
10. customby removing the solvent
11. washwas washed with a diethyl ether-hexane mixed solution

ORD-Eintrag

ord-32633080cc164b10bd5fca74d30a8f21

Quelldatensatz

uspto-grants-1997_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05591752