Hexane → 1,1-Dibromo-2-[2-chloro-4-(methylsulphenyl)phenyl]ethene

Triphenyl phosphine (2.5 g) was added to a stirred solution of carbon tetrabromide (1.48 g) in dichloromethane maintaining the temperature at 0° C. The mixture was stirred for 0.5 hours and 2-chloro-4-(sulphenyl)-benzaldehyde (1.0 g) was added. The resultant mixture was stirred for 0.5 hours and poured into hexane. The resulting solid was filtered off and washed with ether. The combined filtrates were evaporated to dryness and the residue was purified by chromatrography eluted with hexane to give 1,1-dibromo-2-[2-chloro-4-(methylsulphenyl)phenyl]ethene (0.96 g) as a white solid, NMR (CDCl3) 2.45 (s,3H), 7.15(d,1H), 7.25(s,1H), 7.55(s,1H), 7.6(d,1H). By proceeding in a similar manner the following compound was prepared from the appropriately substituted starting material.

1. filtrationThe resulting solid was filtered off
2. washwashed with ether
3. customThe combined filtrates were evaporated to dryness
4. customthe residue was purified by chromatrography
5. washeluted with hexane

ORD-Eintrag

ord-fd964d87592641c1abba733f35d3ef45

Quelldatensatz

uspto-grants-1995_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05424276